# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_2_09s337
_database_code_depnum_ccdc_archive 'CCDC 1962578'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2019-11-14 deposited with the CCDC. 2020-01-23 downloaded from the CCDC.
;
_audit_creation_date 2019-11-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C44 H34 F4 Ir N5 O2, 1.5(C6 H14)'
_chemical_formula_sum 'C53 H55 F4 Ir N5 O2'
_chemical_formula_weight 1062.22
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.7257(3)
_cell_length_b 14.9871(3)
_cell_length_c 15.3105(3)
_cell_angle_alpha 60.9714(6)
_cell_angle_beta 80.3094(7)
_cell_angle_gamma 68.9999(6)
_cell_volume 2383.58(9)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 7131
_cell_measurement_temperature 120
_cell_measurement_theta_max 30.00
_cell_measurement_theta_min 2.30
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.862
_exptl_absorpt_correction_T_max 0.7459
_exptl_absorpt_correction_T_min 0.4919
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Krause et al., 2015) was used for absorption correction.
R(int) was 0.0679 before and 0.0331 after correction. The Ratio
of minimum to maximum transmission is 0.6595. The \l/2 correction
factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.480
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1074
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.08
_exptl_special_details
;
The data collection nominally covered full sphere of reciprocal
space, by a combination of 3 runs of narrow-frame \w-scans (600,
600 and 558 scans, scan width 0.3\% \w, 30s exposure), every run
at a different \f angle. Crystal to detector distance 4.84 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0353
_diffrn_reflns_av_unetI/netI 0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 43033
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 30.006
_diffrn_reflns_theta_min 1.641
_diffrn_ambient_temperature 120
_diffrn_detector 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type 'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART 6000'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_source_current 40.0
_diffrn_source_power 2.0
_diffrn_source_target Mo
_diffrn_source_voltage 50.0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12254
_reflns_number_total 13912
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT version 6.45A (Bruker, 2003)'
_computing_data_collection 'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction 'SAINT version 6.45A (Bruker, 2003)'
_computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_refine_diff_density_max 2.497
_refine_diff_density_min -0.788
_refine_diff_density_rms 0.094
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment refU
_refine_ls_matrix_type full
_refine_ls_number_parameters 533
_refine_ls_number_reflns 13912
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0322
_refine_ls_R_factor_gt 0.0264
_refine_ls_restrained_S_all 1.064
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0676
_refine_ls_wR_factor_ref 0.0700
_refine_special_details
;Methyl groups were refined as rigid bodies rotating around C---C
bonds, with a common refined U for three H atoms. Other H atoms:
riding model.,SQUEEZE
;
_olex2_refinement_description
;
1. Others
Uiso(H20A)=Uiso(H20B)=Uiso(H20C)=FVAR(1)
Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(2)
Uiso(H18A)=Uiso(H18B)=Uiso(H18C)=FVAR(3)
Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(4)
Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(5)
Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(6)
2.a Riding coordinates:
C2(H2), C8(H8), C10(H10), C11(H11), C14(H14), C16(H16), C22(H22), C28(H28),
C30(H30), C31(H31), C34(H34), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46)
2.b Rotating group:
C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B,
H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir Ir 0.36991(2) 0.28286(2) 0.18055(2) 0.02573(3) Uani 1 1 d . . . . .
F1 F 0.03349(15) 0.21657(16) 0.07058(16) 0.0595(5) Uani 1 1 d . . . . .
F2 F -0.05852(14) 0.50617(15) 0.11877(16) 0.0589(5) Uani 1 1 d . . . . .
F3 F 0.27701(18) 0.13097(15) 0.57496(13) 0.0614(5) Uani 1 1 d . . . . .
F4 F 0.43410(17) -0.11259(12) 0.46313(12) 0.0509(4) Uani 1 1 d . . . . .
O1 O 0.40727(15) 0.37896(13) 0.03135(12) 0.0328(4) Uani 1 1 d . . . . .
O2 O 0.54554(18) 0.43258(15) -0.06832(14) 0.0445(5) Uani 1 1 d . . . . .
N1 N 0.28395(17) 0.41836(15) 0.19593(15) 0.0290(4) Uani 1 1 d . . . . .
N2 N 0.44176(16) 0.14360(14) 0.17000(14) 0.0261(4) Uani 1 1 d . . . . .
N3 N 0.53437(16) 0.28063(14) 0.19362(15) 0.0278(4) Uani 1 1 d . . . . .
N4 N -0.0101(2) 0.3608(2) 0.0956(2) 0.0499(6) Uani 1 1 d . . . . .
N24 N 0.3540(2) 0.01104(19) 0.51670(16) 0.0426(5) Uani 1 1 d . . . . .
C1 C 0.2157(2) 0.30412(18) 0.14668(18) 0.0313(5) Uani 1 1 d . . . . .
C2 C 0.1808(2) 0.2414(2) 0.1206(2) 0.0373(5) Uani 1 1 d . . . . .
H2 H 0.232678 0.178159 0.119049 0.033(7) Uiso 1 1 d R . . . .
C3 C 0.0695(3) 0.2751(2) 0.0967(2) 0.0448(6) Uani 1 1 d . . . . .
C5 C 0.0245(2) 0.4194(2) 0.1191(2) 0.0435(6) Uani 1 1 d . . . . .
C6 C 0.1331(2) 0.39861(19) 0.14416(19) 0.0333(5) Uani 1 1 d . . . . .
C7 C 0.1718(2) 0.46335(18) 0.17076(18) 0.0314(5) Uani 1 1 d . . . . .
C8 C 0.1085(2) 0.55897(19) 0.1741(2) 0.0374(5) Uani 1 1 d . . . . .
H8 H 0.031860 0.591347 0.153399 0.039(8) Uiso 1 1 d R . . . .
C9 C 0.1561(2) 0.60837(19) 0.20640(19) 0.0360(5) Uani 1 1 d . . . . .
C10 C 0.2680(2) 0.5584(2) 0.2354(2) 0.0361(5) Uani 1 1 d . . . . .
H10 H 0.302759 0.588034 0.260462 0.056(10) Uiso 1 1 d R . . . .
C11 C 0.3294(2) 0.46554(18) 0.22798(18) 0.0319(5) Uani 1 1 d . . . . .
H11 H 0.406556 0.433288 0.246821 0.040(8) Uiso 1 1 d R . . . .
C12 C 0.0897(2) 0.71004(19) 0.2115(2) 0.0373(6) Uani 1 1 d . . . . .
C13 C 0.0153(3) 0.7080(2) 0.2903(3) 0.0612(10) Uani 1 1 d . . . . .
C14 C -0.0439(3) 0.8034(2) 0.2951(3) 0.0643(11) Uani 1 1 d . . . . .
H14 H -0.093459 0.801125 0.349451 0.103(15) Uiso 1 1 d R . . . .
C15 C -0.0335(3) 0.9007(2) 0.2230(2) 0.0492(7) Uani 1 1 d . . . . .
C16 C 0.0395(3) 0.9019(2) 0.1450(2) 0.0416(6) Uani 1 1 d . . . . .
H16 H 0.048368 0.968522 0.095303 0.035(7) Uiso 1 1 d R . . . .
C17 C 0.1016(2) 0.80832(19) 0.13751(19) 0.0353(5) Uani 1 1 d . . . . .
C18 C -0.0009(5) 0.6029(3) 0.3703(3) 0.109(2) Uani 1 1 d . . . . .
H18A H 0.072345 0.547986 0.396546 0.139(13) Uiso 1 1 d R U . . .
H18B H -0.045903 0.613956 0.425048 0.139(13) Uiso 1 1 d R U . . .
H18C H -0.040466 0.578327 0.340837 0.139(13) Uiso 1 1 d R U . . .
C19 C -0.1036(4) 1.0035(3) 0.2286(3) 0.0683(11) Uani 1 1 d . . . . .
H19A H -0.180377 1.025943 0.205184 0.103(10) Uiso 1 1 d R U . . .
H19B H -0.105940 0.991461 0.297674 0.103(10) Uiso 1 1 d R U . . .
H19C H -0.069705 1.060041 0.186041 0.103(10) Uiso 1 1 d R U . . .
C20 C 0.1777(3) 0.8132(2) 0.0501(2) 0.0485(7) Uani 1 1 d . . . . .
H20A H 0.146374 0.795262 0.008737 0.064(6) Uiso 1 1 d R U . . .
H20B H 0.182945 0.886112 0.010345 0.064(6) Uiso 1 1 d R U . . .
H20C H 0.253116 0.761509 0.073611 0.064(6) Uiso 1 1 d R U . . .
C21 C 0.35373(19) 0.17957(18) 0.32138(17) 0.0283(4) Uani 1 1 d . . . . .
C22 C 0.3103(2) 0.2000(2) 0.40284(19) 0.0356(5) Uani 1 1 d . . . . .
H22 H 0.277798 0.271622 0.394135 0.037(7) Uiso 1 1 d R . . . .
C23 C 0.3153(2) 0.1135(2) 0.4950(2) 0.0416(6) Uani 1 1 d . . . . .
C25 C 0.3937(2) -0.0067(2) 0.43945(19) 0.0368(5) Uani 1 1 d . . . . .
C26 C 0.3983(2) 0.07010(18) 0.34163(17) 0.0293(4) Uani 1 1 d . . . . .
C27 C 0.44624(19) 0.05041(17) 0.25626(17) 0.0282(4) Uani 1 1 d . . . . .
C28 C 0.4898(2) -0.04812(18) 0.25521(18) 0.0319(5) Uani 1 1 d . . . . .
H28 H 0.492977 -0.112159 0.315705 0.038(8) Uiso 1 1 d R . . . .
C29 C 0.5293(2) -0.05442(18) 0.16734(19) 0.0310(5) Uani 1 1 d . . . . .
C30 C 0.5266(2) 0.04187(18) 0.08122(18) 0.0315(5) Uani 1 1 d . . . . .
H30 H 0.555471 0.040803 0.020232 0.042(8) Uiso 1 1 d R . . . .
C31 C 0.4819(2) 0.13820(18) 0.08528(17) 0.0299(5) Uani 1 1 d . . . . .
H31 H 0.478732 0.203143 0.025819 0.031(7) Uiso 1 1 d R . . . .
C32 C 0.5693(2) -0.16030(18) 0.16664(19) 0.0326(5) Uani 1 1 d . . . . .
C33 C 0.4937(2) -0.2176(2) 0.1905(2) 0.0383(6) Uani 1 1 d . . . . .
C34 C 0.5335(2) -0.3195(2) 0.1951(2) 0.0435(6) Uani 1 1 d . . . . .
H34 H 0.482010 -0.357529 0.208957 0.052(9) Uiso 1 1 d R . . . .
C35 C 0.6450(2) -0.3663(2) 0.1787(2) 0.0411(6) Uani 1 1 d . . . . .
C36 C 0.7171(2) -0.3066(2) 0.1518(2) 0.0438(6) Uani 1 1 d . . . . .
H36 H 0.793423 -0.336667 0.137817 0.067(11) Uiso 1 1 d R . . . .
C37 C 0.6814(2) -0.2038(2) 0.1441(2) 0.0398(6) Uani 1 1 d . . . . .
C38 C 0.3695(3) -0.1707(3) 0.2074(3) 0.0540(8) Uani 1 1 d . . . . .
H38A H 0.341097 -0.094898 0.157307 0.058(6) Uiso 1 1 d R U . . .
H38B H 0.327977 -0.211568 0.201878 0.058(6) Uiso 1 1 d R U . . .
H38C H 0.359187 -0.175537 0.274267 0.058(6) Uiso 1 1 d R U . . .
C39 C 0.6866(3) -0.4794(2) 0.1902(3) 0.0546(8) Uani 1 1 d . . . . .
H39A H 0.743895 -0.526351 0.243432 0.097(9) Uiso 1 1 d R U . . .
H39B H 0.623446 -0.507943 0.207074 0.097(9) Uiso 1 1 d R U . . .
H39C H 0.719909 -0.478009 0.127041 0.097(9) Uiso 1 1 d R U . . .
C40 C 0.7642(3) -0.1422(3) 0.1128(4) 0.0682(11) Uani 1 1 d . . . . .
H40A H 0.758043 -0.108728 0.156041 0.101(9) Uiso 1 1 d R U . . .
H40B H 0.841617 -0.191798 0.117705 0.101(9) Uiso 1 1 d R U . . .
H40C H 0.749162 -0.084731 0.043045 0.101(9) Uiso 1 1 d R U . . .
C41 C 0.5064(2) 0.38685(18) 0.01456(18) 0.0325(5) Uani 1 1 d . . . . .
C42 C 0.5804(2) 0.33341(17) 0.10531(18) 0.0312(5) Uani 1 1 d . . . . .
C43 C 0.6889(2) 0.3367(2) 0.0998(2) 0.0381(6) Uani 1 1 d . . . . .
H43 H 0.719472 0.375256 0.037269 0.054(10) Uiso 1 1 d R . . . .
C44 C 0.7521(2) 0.2840(2) 0.1853(2) 0.0436(7) Uani 1 1 d . . . . .
H44 H 0.826540 0.285413 0.183072 0.039(8) Uiso 1 1 d R . . . .
C45 C 0.7056(2) 0.2282(2) 0.2756(2) 0.0410(6) Uani 1 1 d . . . . .
H45 H 0.748031 0.190430 0.335792 0.050(9) Uiso 1 1 d R . . . .
C46 C 0.5966(2) 0.22834(19) 0.27747(19) 0.0340(5) Uani 1 1 d . . . . .
H46 H 0.565014 0.189982 0.339591 0.043(8) Uiso 1 1 d R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir 0.02647(5) 0.01692(4) 0.03105(5) -0.01154(3) 0.00678(3) -0.00628(3)
F1 0.0457(10) 0.0584(12) 0.0941(15) -0.0465(11) -0.0040(10) -0.0197(9)
F2 0.0306(8) 0.0497(11) 0.0959(15) -0.0420(11) -0.0002(9) 0.0002(7)
F3 0.0809(14) 0.0509(11) 0.0394(9) -0.0225(8) 0.0250(9) -0.0159(10)
F4 0.0762(12) 0.0243(7) 0.0391(8) -0.0085(6) 0.0056(8) -0.0132(8)
O1 0.0413(10) 0.0210(7) 0.0319(8) -0.0116(6) 0.0078(7) -0.0096(7)
O2 0.0609(13) 0.0344(10) 0.0367(9) -0.0158(8) 0.0200(9) -0.0232(9)
N1 0.0298(10) 0.0204(8) 0.0332(9) -0.0131(7) 0.0093(7) -0.0071(7)
N2 0.0258(9) 0.0192(8) 0.0313(9) -0.0120(7) 0.0033(7) -0.0060(7)
N3 0.0272(9) 0.0180(8) 0.0370(10) -0.0142(7) 0.0086(7) -0.0077(7)
N4 0.0328(12) 0.0461(14) 0.0724(18) -0.0301(13) 0.0006(11) -0.0105(11)
N24 0.0486(13) 0.0347(12) 0.0347(11) -0.0109(9) 0.0085(9) -0.0139(10)
C1 0.0306(11) 0.0231(10) 0.0369(12) -0.0134(9) 0.0045(9) -0.0077(9)
C2 0.0338(12) 0.0279(12) 0.0494(14) -0.0191(11) 0.0046(11) -0.0092(10)
C3 0.0403(15) 0.0414(15) 0.0608(18) -0.0269(13) 0.0028(13) -0.0179(12)
C5 0.0297(13) 0.0364(14) 0.0593(17) -0.0235(13) 0.0048(11) -0.0050(11)
C6 0.0290(11) 0.0256(11) 0.0425(13) -0.0164(10) 0.0059(9) -0.0071(9)
C7 0.0308(11) 0.0235(10) 0.0355(11) -0.0135(9) 0.0074(9) -0.0072(9)
C8 0.0344(13) 0.0237(11) 0.0455(14) -0.0161(10) 0.0058(10) -0.0025(9)
C9 0.0421(14) 0.0205(10) 0.0398(13) -0.0149(9) 0.0156(10) -0.0095(10)
C10 0.0407(14) 0.0274(11) 0.0433(13) -0.0205(10) 0.0144(11) -0.0144(10)
C11 0.0331(12) 0.0240(10) 0.0389(12) -0.0173(9) 0.0099(9) -0.0097(9)
C12 0.0416(14) 0.0235(11) 0.0415(13) -0.0169(10) 0.0114(11) -0.0070(10)
C13 0.079(2) 0.0262(13) 0.0569(18) -0.0181(13) 0.0350(17) -0.0099(14)
C14 0.082(2) 0.0312(14) 0.0571(19) -0.0219(14) 0.0352(17) -0.0074(15)
C15 0.0619(19) 0.0267(13) 0.0526(16) -0.0236(12) 0.0095(14) -0.0038(12)
C16 0.0534(16) 0.0235(11) 0.0456(14) -0.0174(11) 0.0070(12) -0.0109(11)
C17 0.0393(13) 0.0249(11) 0.0402(13) -0.0163(10) 0.0077(10) -0.0100(10)
C18 0.153(5) 0.0332(17) 0.093(3) -0.0241(19) 0.087(3) -0.024(2)
C19 0.093(3) 0.0308(15) 0.068(2) -0.0294(15) 0.018(2) -0.0038(16)
C20 0.0605(19) 0.0308(13) 0.0476(15) -0.0178(12) 0.0191(14) -0.0163(13)
C21 0.0242(10) 0.0255(10) 0.0348(11) -0.0139(9) 0.0051(8) -0.0098(8)
C22 0.0384(13) 0.0295(12) 0.0363(12) -0.0168(10) 0.0104(10) -0.0103(10)
C23 0.0418(14) 0.0422(15) 0.0354(13) -0.0179(11) 0.0122(11) -0.0128(12)
C25 0.0383(13) 0.0261(11) 0.0375(13) -0.0088(10) 0.0019(10) -0.0105(10)
C26 0.0288(11) 0.0246(10) 0.0317(11) -0.0109(9) 0.0040(8) -0.0101(9)
C27 0.0278(11) 0.0197(9) 0.0345(11) -0.0112(8) 0.0004(8) -0.0068(8)
C28 0.0342(12) 0.0175(9) 0.0391(12) -0.0104(9) -0.0021(9) -0.0060(9)
C29 0.0286(11) 0.0215(10) 0.0433(13) -0.0171(9) -0.0033(9) -0.0038(8)
C30 0.0332(12) 0.0248(11) 0.0367(12) -0.0168(9) 0.0020(9) -0.0066(9)
C31 0.0333(12) 0.0224(10) 0.0325(11) -0.0126(9) 0.0038(9) -0.0091(9)
C32 0.0336(12) 0.0205(10) 0.0426(13) -0.0160(9) -0.0049(10) -0.0029(9)
C33 0.0373(13) 0.0259(11) 0.0524(15) -0.0208(11) 0.0008(11) -0.0073(10)
C34 0.0445(15) 0.0277(12) 0.0630(18) -0.0243(12) -0.0005(13) -0.0114(11)
C35 0.0454(15) 0.0258(12) 0.0540(16) -0.0226(11) -0.0082(12) -0.0035(11)
C36 0.0364(14) 0.0288(12) 0.0640(18) -0.0254(13) -0.0048(12) -0.0002(10)
C37 0.0345(13) 0.0251(11) 0.0571(16) -0.0210(11) -0.0018(11) -0.0028(10)
C38 0.0392(15) 0.0420(16) 0.089(2) -0.0386(17) 0.0104(15) -0.0149(13)
C39 0.0582(19) 0.0270(13) 0.079(2) -0.0302(14) -0.0109(16) -0.0002(13)
C40 0.0361(16) 0.0438(18) 0.127(3) -0.047(2) 0.0097(18) -0.0088(14)
C41 0.0427(13) 0.0196(10) 0.0349(11) -0.0155(9) 0.0117(10) -0.0106(9)
C42 0.0361(12) 0.0184(9) 0.0403(12) -0.0176(9) 0.0130(10) -0.0098(9)
C43 0.0348(13) 0.0272(11) 0.0556(16) -0.0248(11) 0.0190(11) -0.0136(10)
C44 0.0296(12) 0.0300(12) 0.077(2) -0.0321(13) 0.0118(13) -0.0109(10)
C45 0.0363(13) 0.0301(12) 0.0586(17) -0.0220(12) -0.0002(12) -0.0106(11)
C46 0.0344(12) 0.0242(11) 0.0414(13) -0.0137(10) 0.0031(10) -0.0105(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir O1 2.1096(16) . ?
Ir N1 2.0398(19) . ?
Ir N2 2.0317(18) . ?
Ir N3 2.123(2) . ?
Ir C1 1.989(3) . ?
Ir C21 1.982(2) . ?
F1 C3 1.352(3) . ?
F2 C5 1.348(3) . ?
F3 C23 1.350(3) . ?
F4 C25 1.355(3) . ?
O1 C41 1.281(3) . ?
O2 C41 1.231(3) . ?
N1 C7 1.372(3) . ?
N1 C11 1.342(3) . ?
N2 C27 1.370(3) . ?
N2 C31 1.341(3) . ?
N3 C42 1.351(3) . ?
N3 C46 1.346(3) . ?
N4 C3 1.315(4) . ?
N4 C5 1.316(4) . ?
N24 C23 1.316(4) . ?
N24 C25 1.316(4) . ?
C1 C2 1.400(4) . ?
C1 C6 1.416(3) . ?
C2 H2 0.9501 . ?
C2 C3 1.371(4) . ?
C5 C6 1.381(4) . ?
C6 C7 1.464(3) . ?
C7 C8 1.391(3) . ?
C8 H8 0.9497 . ?
C8 C9 1.392(4) . ?
C9 C10 1.383(4) . ?
C9 C12 1.488(3) . ?
C10 H10 0.9504 . ?
C10 C11 1.380(3) . ?
C11 H11 0.9496 . ?
C12 C13 1.397(4) . ?
C12 C17 1.400(3) . ?
C13 C14 1.389(4) . ?
C13 C18 1.516(4) . ?
C14 H14 0.9503 . ?
C14 C15 1.374(4) . ?
C15 C16 1.381(4) . ?
C15 C19 1.515(4) . ?
C16 H16 0.9501 . ?
C16 C17 1.392(3) . ?
C17 C20 1.501(4) . ?
C18 H18A 0.9815 . ?
C18 H18B 0.9812 . ?
C18 H18C 0.9816 . ?
C19 H19A 0.9810 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9796 . ?
C20 H20A 0.9799 . ?
C20 H20B 0.9806 . ?
C20 H20C 0.9812 . ?
C21 C22 1.404(3) . ?
C21 C26 1.417(3) . ?
C22 H22 0.9499 . ?
C22 C23 1.368(4) . ?
C25 C26 1.384(3) . ?
C26 C27 1.465(3) . ?
C27 C28 1.386(3) . ?
C28 H28 0.9502 . ?
C28 C29 1.390(4) . ?
C29 C30 1.398(3) . ?
C29 C32 1.488(3) . ?
C30 H30 0.9499 . ?
C30 C31 1.378(3) . ?
C31 H31 0.9498 . ?
C32 C33 1.402(4) . ?
C32 C37 1.401(4) . ?
C33 C34 1.396(3) . ?
C33 C38 1.517(4) . ?
C34 H34 0.9499 . ?
C34 C35 1.380(4) . ?
C35 C36 1.384(4) . ?
C35 C39 1.511(4) . ?
C36 H36 0.9497 . ?
C36 C37 1.391(4) . ?
C37 C40 1.512(4) . ?
C38 H38A 0.9813 . ?
C38 H38B 0.9796 . ?
C38 H38C 0.9799 . ?
C39 H39A 0.9833 . ?
C39 H39B 0.9829 . ?
C39 H39C 0.9814 . ?
C40 H40A 0.9869 . ?
C40 H40B 0.9873 . ?
C40 H40C 0.9887 . ?
C41 C42 1.509(4) . ?
C42 C43 1.385(4) . ?
C43 H43 0.9494 . ?
C43 C44 1.371(4) . ?
C44 H44 0.9503 . ?
C44 C45 1.384(4) . ?
C45 H45 0.9509 . ?
C45 C46 1.381(4) . ?
C46 H46 0.9504 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ir N3 77.72(7) . . ?
N1 Ir O1 89.98(7) . . ?
N1 Ir N3 97.09(8) . . ?
N2 Ir O1 93.35(7) . . ?
N2 Ir N1 174.40(7) . . ?
N2 Ir N3 88.03(7) . . ?
C1 Ir O1 93.43(8) . . ?
C1 Ir N1 80.61(9) . . ?
C1 Ir N2 94.68(9) . . ?
C1 Ir N3 170.90(8) . . ?
C21 Ir O1 172.84(8) . . ?
C21 Ir N1 95.84(8) . . ?
C21 Ir N2 81.19(9) . . ?
C21 Ir N3 97.36(8) . . ?
C21 Ir C1 91.64(9) . . ?
C41 O1 Ir 116.66(16) . . ?
C7 N1 Ir 116.49(16) . . ?
C11 N1 Ir 124.75(16) . . ?
C11 N1 C7 118.8(2) . . ?
C27 N2 Ir 116.17(15) . . ?
C31 N2 Ir 124.49(15) . . ?
C31 N2 C27 119.32(19) . . ?
C42 N3 Ir 113.82(17) . . ?
C46 N3 Ir 127.17(15) . . ?
C46 N3 C42 118.9(2) . . ?
C3 N4 C5 114.4(3) . . ?
C23 N24 C25 114.2(2) . . ?
C2 C1 Ir 128.47(18) . . ?
C2 C1 C6 117.1(2) . . ?
C6 C1 Ir 114.33(18) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 C1 117.6(2) . . ?
C3 C2 H2 121.3 . . ?
F1 C3 C2 118.9(3) . . ?
N4 C3 F1 113.9(3) . . ?
N4 C3 C2 127.2(3) . . ?
F2 C5 C6 120.0(3) . . ?
N4 C5 F2 113.5(2) . . ?
N4 C5 C6 126.5(3) . . ?
C1 C6 C7 116.1(2) . . ?
C5 C6 C1 117.3(2) . . ?
C5 C6 C7 126.6(2) . . ?
N1 C7 C6 112.3(2) . . ?
N1 C7 C8 120.1(2) . . ?
C8 C7 C6 127.6(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 120.9(2) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 C12 121.9(2) . . ?
C10 C9 C8 117.5(2) . . ?
C10 C9 C12 120.7(2) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.1(2) . . ?
C11 C10 H10 119.9 . . ?
N1 C11 C10 122.5(2) . . ?
N1 C11 H11 118.6 . . ?
C10 C11 H11 118.9 . . ?
C13 C12 C9 120.2(2) . . ?
C13 C12 C17 119.6(2) . . ?
C17 C12 C9 120.1(2) . . ?
C12 C13 C18 120.7(3) . . ?
C14 C13 C12 119.4(3) . . ?
C14 C13 C18 119.9(3) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 C13 121.8(3) . . ?
C15 C14 H14 119.3 . . ?
C14 C15 C16 118.3(3) . . ?
C14 C15 C19 120.2(3) . . ?
C16 C15 C19 121.5(3) . . ?
C15 C16 H16 119.1 . . ?
C15 C16 C17 122.0(2) . . ?
C17 C16 H16 118.9 . . ?
C12 C17 C20 120.7(2) . . ?
C16 C17 C12 118.8(2) . . ?
C16 C17 C20 120.5(2) . . ?
C13 C18 H18A 110.2 . . ?
C13 C18 H18B 109.9 . . ?
C13 C18 H18C 108.8 . . ?
H18A C18 H18B 109.3 . . ?
H18A C18 H18C 109.3 . . ?
H18B C18 H18C 109.3 . . ?
C15 C19 H19A 109.6 . . ?
C15 C19 H19B 109.9 . . ?
C15 C19 H19C 109.1 . . ?
H19A C19 H19B 109.4 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 108.9 . . ?
C17 C20 H20B 109.6 . . ?
C17 C20 H20C 110.1 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.4 . . ?
H20B C20 H20C 109.4 . . ?
C22 C21 Ir 129.02(18) . . ?
C22 C21 C26 116.8(2) . . ?
C26 C21 Ir 114.03(17) . . ?
C21 C22 H22 121.1 . . ?
C23 C22 C21 117.9(2) . . ?
C23 C22 H22 121.0 . . ?
F3 C23 C22 119.1(3) . . ?
N24 C23 F3 113.8(2) . . ?
N24 C23 C22 127.1(3) . . ?
F4 C25 C26 119.8(2) . . ?
N24 C25 F4 113.4(2) . . ?
N24 C25 C26 126.8(2) . . ?
C21 C26 C27 115.99(19) . . ?
C25 C26 C21 117.1(2) . . ?
C25 C26 C27 126.9(2) . . ?
N2 C27 C26 112.59(19) . . ?
N2 C27 C28 120.1(2) . . ?
C28 C27 C26 127.3(2) . . ?
C27 C28 H28 119.2 . . ?
C27 C28 C29 121.0(2) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C30 117.4(2) . . ?
C28 C29 C32 120.1(2) . . ?
C30 C29 C32 122.4(2) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 C29 119.7(2) . . ?
C31 C30 H30 120.2 . . ?
N2 C31 C30 122.3(2) . . ?
N2 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
C33 C32 C29 119.2(2) . . ?
C37 C32 C29 120.9(2) . . ?
C37 C32 C33 119.9(2) . . ?
C32 C33 C38 122.2(2) . . ?
C34 C33 C32 118.7(2) . . ?
C34 C33 C38 119.0(2) . . ?
C33 C34 H34 118.9 . . ?
C35 C34 C33 122.1(3) . . ?
C35 C34 H34 118.9 . . ?
C34 C35 C36 118.0(2) . . ?
C34 C35 C39 120.8(3) . . ?
C36 C35 C39 121.2(3) . . ?
C35 C36 H36 119.0 . . ?
C35 C36 C37 122.2(3) . . ?
C37 C36 H36 118.9 . . ?
C32 C37 C40 121.7(2) . . ?
C36 C37 C32 118.9(2) . . ?
C36 C37 C40 119.5(3) . . ?
C33 C38 H38A 109.9 . . ?
C33 C38 H38B 109.3 . . ?
C33 C38 H38C 109.3 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.3 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39A 110.1 . . ?
C35 C39 H39B 109.8 . . ?
C35 C39 H39C 109.3 . . ?
H39A C39 H39B 109.3 . . ?
H39A C39 H39C 109.2 . . ?
H39B C39 H39C 109.2 . . ?
C37 C40 H40A 110.8 . . ?
C37 C40 H40B 109.7 . . ?
C37 C40 H40C 110.2 . . ?
H40A C40 H40B 108.8 . . ?
H40A C40 H40C 108.4 . . ?
H40B C40 H40C 108.9 . . ?
O1 C41 C42 116.0(2) . . ?
O2 C41 O1 125.5(3) . . ?
O2 C41 C42 118.4(2) . . ?
N3 C42 C41 115.6(2) . . ?
N3 C42 C43 121.4(2) . . ?
C43 C42 C41 123.0(2) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 C42 119.7(2) . . ?
C44 C43 H43 120.0 . . ?
C43 C44 H44 120.9 . . ?
C43 C44 C45 118.9(3) . . ?
C45 C44 H44 120.2 . . ?
C44 C45 H45 120.4 . . ?
C46 C45 C44 119.4(3) . . ?
C46 C45 H45 120.2 . . ?
N3 C46 C45 121.8(2) . . ?
N3 C46 H46 119.1 . . ?
C45 C46 H46 119.1 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ir O1 C41 O2 174.31(19) . . . . ?
Ir O1 C41 C42 -4.7(2) . . . . ?
Ir N1 C7 C6 4.4(3) . . . . ?
Ir N1 C7 C8 -176.67(18) . . . . ?
Ir N1 C11 C10 178.81(18) . . . . ?
Ir N2 C27 C26 -0.7(2) . . . . ?
Ir N2 C27 C28 177.49(17) . . . . ?
Ir N2 C31 C30 -177.81(18) . . . . ?
Ir N3 C42 C41 1.8(2) . . . . ?
Ir N3 C42 C43 -177.69(17) . . . . ?
Ir N3 C46 C45 176.29(18) . . . . ?
Ir C1 C2 C3 -177.6(2) . . . . ?
Ir C1 C6 C5 178.7(2) . . . . ?
Ir C1 C6 C7 -2.6(3) . . . . ?
Ir C21 C22 C23 -175.5(2) . . . . ?
Ir C21 C26 C25 177.56(18) . . . . ?
Ir C21 C26 C27 -1.4(3) . . . . ?
F2 C5 C6 C1 177.8(2) . . . . ?
F2 C5 C6 C7 -0.8(4) . . . . ?
F4 C25 C26 C21 179.4(2) . . . . ?
F4 C25 C26 C27 -1.8(4) . . . . ?
O1 C41 C42 N3 1.9(3) . . . . ?
O1 C41 C42 C43 -178.6(2) . . . . ?
O2 C41 C42 N3 -177.2(2) . . . . ?
O2 C41 C42 C43 2.3(3) . . . . ?
N1 C7 C8 C9 -2.4(4) . . . . ?
N2 C27 C28 C29 -0.2(4) . . . . ?
N3 C42 C43 C44 1.1(4) . . . . ?
N4 C5 C6 C1 -1.2(5) . . . . ?
N4 C5 C6 C7 -179.7(3) . . . . ?
N24 C25 C26 C21 -1.3(4) . . . . ?
N24 C25 C26 C27 177.5(3) . . . . ?
C1 C2 C3 F1 179.6(3) . . . . ?
C1 C2 C3 N4 -0.3(5) . . . . ?
C1 C6 C7 N1 -1.2(3) . . . . ?
C1 C6 C7 C8 180.0(2) . . . . ?
C2 C1 C6 C5 1.9(4) . . . . ?
C2 C1 C6 C7 -179.4(2) . . . . ?
C3 N4 C5 F2 -179.3(3) . . . . ?
C3 N4 C5 C6 -0.3(5) . . . . ?
C5 N4 C3 F1 -178.8(3) . . . . ?
C5 N4 C3 C2 1.1(5) . . . . ?
C5 C6 C7 N1 177.4(2) . . . . ?
C5 C6 C7 C8 -1.5(4) . . . . ?
C6 C1 C2 C3 -1.3(4) . . . . ?
C6 C7 C8 C9 176.3(2) . . . . ?
C7 N1 C11 C10 -0.9(3) . . . . ?
C7 C8 C9 C10 -0.4(4) . . . . ?
C7 C8 C9 C12 -179.4(2) . . . . ?
C8 C9 C10 C11 2.6(4) . . . . ?
C8 C9 C12 C13 77.6(4) . . . . ?
C8 C9 C12 C17 -102.5(3) . . . . ?
C9 C10 C11 N1 -2.0(4) . . . . ?
C9 C12 C13 C14 178.5(4) . . . . ?
C9 C12 C13 C18 -1.3(6) . . . . ?
C9 C12 C17 C16 -179.2(3) . . . . ?
C9 C12 C17 C20 2.4(4) . . . . ?
C10 C9 C12 C13 -101.3(4) . . . . ?
C10 C9 C12 C17 78.6(4) . . . . ?
C11 N1 C7 C6 -175.9(2) . . . . ?
C11 N1 C7 C8 3.0(3) . . . . ?
C12 C9 C10 C11 -178.4(2) . . . . ?
C12 C13 C14 C15 1.6(7) . . . . ?
C13 C12 C17 C16 0.7(5) . . . . ?
C13 C12 C17 C20 -177.7(3) . . . . ?
C13 C14 C15 C16 -1.0(6) . . . . ?
C13 C14 C15 C19 177.2(4) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C15 C16 C17 C12 -0.2(5) . . . . ?
C15 C16 C17 C20 178.2(3) . . . . ?
C17 C12 C13 C14 -1.4(6) . . . . ?
C17 C12 C13 C18 178.8(4) . . . . ?
C18 C13 C14 C15 -178.6(5) . . . . ?
C19 C15 C16 C17 -177.9(3) . . . . ?
C21 C22 C23 F3 178.2(2) . . . . ?
C21 C22 C23 N24 -2.1(5) . . . . ?
C21 C26 C27 N2 1.4(3) . . . . ?
C21 C26 C27 C28 -176.7(2) . . . . ?
C22 C21 C26 C25 0.8(3) . . . . ?
C22 C21 C26 C27 -178.2(2) . . . . ?
C23 N24 C25 F4 179.5(2) . . . . ?
C23 N24 C25 C26 0.1(4) . . . . ?
C25 N24 C23 F3 -178.6(2) . . . . ?
C25 N24 C23 C22 1.7(5) . . . . ?
C25 C26 C27 N2 -177.5(2) . . . . ?
C25 C26 C27 C28 4.5(4) . . . . ?
C26 C21 C22 C23 0.7(4) . . . . ?
C26 C27 C28 C29 177.7(2) . . . . ?
C27 N2 C31 C30 0.8(3) . . . . ?
C27 C28 C29 C30 2.0(4) . . . . ?
C27 C28 C29 C32 -176.3(2) . . . . ?
C28 C29 C30 C31 -2.4(4) . . . . ?
C28 C29 C32 C33 61.7(3) . . . . ?
C28 C29 C32 C37 -117.3(3) . . . . ?
C29 C30 C31 N2 1.0(4) . . . . ?
C29 C32 C33 C34 -176.5(3) . . . . ?
C29 C32 C33 C38 6.0(4) . . . . ?
C29 C32 C37 C36 175.1(3) . . . . ?
C29 C32 C37 C40 -4.2(4) . . . . ?
C30 C29 C32 C33 -116.5(3) . . . . ?
C30 C29 C32 C37 64.5(3) . . . . ?
C31 N2 C27 C26 -179.5(2) . . . . ?
C31 N2 C27 C28 -1.2(3) . . . . ?
C32 C29 C30 C31 175.8(2) . . . . ?
C32 C33 C34 C35 1.2(4) . . . . ?
C33 C32 C37 C36 -3.8(4) . . . . ?
C33 C32 C37 C40 176.8(3) . . . . ?
C33 C34 C35 C36 -3.4(5) . . . . ?
C33 C34 C35 C39 176.4(3) . . . . ?
C34 C35 C36 C37 2.0(5) . . . . ?
C35 C36 C37 C32 1.6(5) . . . . ?
C35 C36 C37 C40 -179.0(3) . . . . ?
C37 C32 C33 C34 2.5(4) . . . . ?
C37 C32 C33 C38 -175.0(3) . . . . ?
C38 C33 C34 C35 178.8(3) . . . . ?
C39 C35 C36 C37 -177.8(3) . . . . ?
C41 C42 C43 C44 -178.4(2) . . . . ?
C42 N3 C46 C45 0.6(3) . . . . ?
C42 C43 C44 C45 0.2(4) . . . . ?
C43 C44 C45 C46 -1.0(4) . . . . ?
C44 C45 C46 N3 0.6(4) . . . . ?
C46 N3 C42 C41 178.1(2) . . . . ?
C46 N3 C42 C43 -1.5(3) . . . . ?
_smtbx_masks_special_details
;
A solvent mask was calculated (Rees et al., 2005) and 151 electrons were
found in the volume of 705\%A^3^ in 1 void per unit cell. This is consistent
with the presence of 1.5 molecules of hexane (C~6~H~14~) per Formula Unit,
which account for 150 electrons per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.560 0.371 0.500 704.9 150.9 '3 hexane molecules'
_smtbx_masks_void_probe_radius 1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_file
;
TITL 09SRV337 OLEX2: imported from CIF
09srv337.res
created by SHELXL-2018/3 at 15:34:00 on 14-Nov-2019
CELL 0.71073 12.7257 14.9871 15.3105 60.9714 80.3094 68.9999
ZERR 2 0.0003 0.0003 0.0003 0.0006 0.0007 0.0006
LATT 1
SFAC C F H Ir N O
UNIT 106 8 110 2 10 4
L.S. 7 0 85
PLAN 17
TEMP -153.15
CONF
MORE -1
BOND $H
ABIN
fmap 2 53
acta 60
OMIT 5 6 1
OMIT 0 0 1
OMIT 0 -1 1
REM
REM
REM
WGHT 0.038100 0.085700
FVAR 0.25570 0.06431 0.10274 0.13914 0.10091 0.09670 0.05834
IR 4 0.369913 0.282864 0.180545 11.00000 0.02647 0.01692 =
0.03105 -0.01154 0.00678 -0.00628
F1 2 0.033485 0.216573 0.070579 11.00000 0.04566 0.05845 =
0.09414 -0.04653 -0.00404 -0.01971
F2 2 -0.058517 0.506172 0.118767 11.00000 0.03063 0.04968 =
0.09586 -0.04198 -0.00025 0.00024
F3 2 0.277010 0.130970 0.574961 11.00000 0.08091 0.05094 =
0.03936 -0.02247 0.02503 -0.01588
F4 2 0.434101 -0.112593 0.463135 11.00000 0.07615 0.02433 =
0.03906 -0.00853 0.00561 -0.01323
O1 6 0.407272 0.378962 0.031352 11.00000 0.04132 0.02099 =
0.03189 -0.01164 0.00785 -0.00962
O2 6 0.545535 0.432575 -0.068324 11.00000 0.06090 0.03440 =
0.03671 -0.01582 0.02001 -0.02322
N1 5 0.283954 0.418357 0.195925 11.00000 0.02984 0.02037 =
0.03319 -0.01314 0.00929 -0.00712
N2 5 0.441758 0.143601 0.170003 11.00000 0.02580 0.01921 =
0.03129 -0.01198 0.00331 -0.00602
N3 5 0.534368 0.280634 0.193617 11.00000 0.02717 0.01803 =
0.03704 -0.01422 0.00864 -0.00766
N4 5 -0.010140 0.360785 0.095621 11.00000 0.03276 0.04609 =
0.07238 -0.03007 0.00056 -0.01052
N24 5 0.354023 0.011040 0.516700 11.00000 0.04860 0.03473 =
0.03471 -0.01086 0.00851 -0.01389
C1 1 0.215664 0.304120 0.146685 11.00000 0.03058 0.02310 =
0.03694 -0.01341 0.00450 -0.00774
C2 1 0.180848 0.241419 0.120589 11.00000 0.03378 0.02795 =
0.04943 -0.01910 0.00464 -0.00924
AFIX 3
H2 3 0.232678 0.178159 0.119049 11.00000 0.03259
AFIX 0
C3 1 0.069487 0.275107 0.096661 11.00000 0.04028 0.04144 =
0.06076 -0.02694 0.00276 -0.01795
C5 1 0.024475 0.419387 0.119118 11.00000 0.02967 0.03640 =
0.05934 -0.02350 0.00483 -0.00499
C6 1 0.133069 0.398610 0.144162 11.00000 0.02904 0.02556 =
0.04248 -0.01642 0.00595 -0.00710
C7 1 0.171812 0.463355 0.170756 11.00000 0.03078 0.02348 =
0.03548 -0.01354 0.00740 -0.00718
C8 1 0.108450 0.558967 0.174139 11.00000 0.03437 0.02373 =
0.04546 -0.01608 0.00581 -0.00245
AFIX 3
H8 3 0.031860 0.591347 0.153399 11.00000 0.03861
AFIX 0
C9 1 0.156051 0.608373 0.206400 11.00000 0.04211 0.02052 =
0.03981 -0.01485 0.01565 -0.00953
C10 1 0.267969 0.558414 0.235422 11.00000 0.04074 0.02738 =
0.04327 -0.02049 0.01435 -0.01440
AFIX 3
H10 3 0.302759 0.588034 0.260462 11.00000 0.05650
AFIX 0
C11 1 0.329356 0.465538 0.227981 11.00000 0.03313 0.02405 =
0.03892 -0.01730 0.00991 -0.00974
AFIX 3
H11 3 0.406556 0.433288 0.246821 11.00000 0.03954
AFIX 0
C12 1 0.089684 0.710039 0.211539 11.00000 0.04160 0.02355 =
0.04147 -0.01693 0.01143 -0.00702
C13 1 0.015270 0.708012 0.290255 11.00000 0.07851 0.02618 =
0.05689 -0.01809 0.03503 -0.00985
C14 1 -0.043929 0.803395 0.295061 11.00000 0.08221 0.03119 =
0.05706 -0.02185 0.03522 -0.00741
AFIX 3
H14 3 -0.093459 0.801125 0.349451 11.00000 0.10255
AFIX 0
C15 1 -0.033520 0.900665 0.223036 11.00000 0.06188 0.02672 =
0.05263 -0.02360 0.00955 -0.00385
C16 1 0.039538 0.901922 0.145043 11.00000 0.05340 0.02353 =
0.04556 -0.01737 0.00704 -0.01091
AFIX 3
H16 3 0.048368 0.968522 0.095303 11.00000 0.03542
AFIX 0
C17 1 0.101648 0.808319 0.137512 11.00000 0.03935 0.02485 =
0.04018 -0.01630 0.00766 -0.00999
C18 1 -0.000915 0.602917 0.370307 11.00000 0.15256 0.03318 =
0.09277 -0.02414 0.08744 -0.02364
AFIX 7
H18A 3 0.072345 0.547986 0.396546 11.00000 41.00000
H18B 3 -0.045903 0.613956 0.425048 11.00000 41.00000
H18C 3 -0.040466 0.578327 0.340837 11.00000 41.00000
AFIX 0
C19 1 -0.103560 1.003495 0.228583 11.00000 0.09317 0.03076 =
0.06764 -0.02941 0.01815 -0.00375
AFIX 7
H19A 3 -0.180377 1.025943 0.205184 11.00000 31.00000
H19B 3 -0.105940 0.991461 0.297674 11.00000 31.00000
H19C 3 -0.069705 1.060041 0.186041 11.00000 31.00000
AFIX 0
C20 1 0.177749 0.813204 0.050101 11.00000 0.06051 0.03083 =
0.04763 -0.01780 0.01911 -0.01633
AFIX 7
H20A 3 0.146374 0.795262 0.008737 11.00000 21.00000
H20B 3 0.182945 0.886112 0.010345 11.00000 21.00000
H20C 3 0.253116 0.761509 0.073611 11.00000 21.00000
AFIX 0
C21 1 0.353734 0.179567 0.321380 11.00000 0.02416 0.02554 =
0.03482 -0.01387 0.00512 -0.00975
C22 1 0.310338 0.200012 0.402845 11.00000 0.03841 0.02949 =
0.03632 -0.01677 0.01041 -0.01026
AFIX 3
H22 3 0.277798 0.271622 0.394135 11.00000 0.03665
AFIX 0
C23 1 0.315342 0.113547 0.495041 11.00000 0.04178 0.04218 =
0.03541 -0.01793 0.01216 -0.01280
C25 1 0.393737 -0.006668 0.439452 11.00000 0.03826 0.02608 =
0.03751 -0.00875 0.00189 -0.01049
C26 1 0.398257 0.070104 0.341626 11.00000 0.02885 0.02456 =
0.03175 -0.01094 0.00396 -0.01013
C27 1 0.446238 0.050407 0.256255 11.00000 0.02777 0.01967 =
0.03452 -0.01125 0.00039 -0.00679
C28 1 0.489837 -0.048119 0.255215 11.00000 0.03424 0.01755 =
0.03914 -0.01039 -0.00212 -0.00604
AFIX 3
H28 3 0.492977 -0.112159 0.315705 11.00000 0.03789
AFIX 0
C29 1 0.529328 -0.054419 0.167339 11.00000 0.02858 0.02152 =
0.04329 -0.01707 -0.00334 -0.00378
C30 1 0.526551 0.041873 0.081222 11.00000 0.03322 0.02479 =
0.03669 -0.01680 0.00204 -0.00658
AFIX 3
H30 3 0.555471 0.040803 0.020232 11.00000 0.04166
AFIX 0
C31 1 0.481852 0.138203 0.085279 11.00000 0.03330 0.02244 =
0.03254 -0.01262 0.00375 -0.00909
AFIX 3
H31 3 0.478732 0.203143 0.025819 11.00000 0.03138
AFIX 0
C32 1 0.569335 -0.160297 0.166640 11.00000 0.03359 0.02053 =
0.04255 -0.01602 -0.00492 -0.00293
C33 1 0.493750 -0.217625 0.190500 11.00000 0.03731 0.02594 =
0.05241 -0.02078 0.00078 -0.00729
C34 1 0.533540 -0.319549 0.195067 11.00000 0.04452 0.02768 =
0.06301 -0.02434 -0.00051 -0.01142
AFIX 3
H34 3 0.482010 -0.357529 0.208957 11.00000 0.05186
AFIX 0
C35 1 0.644973 -0.366264 0.178667 11.00000 0.04537 0.02583 =
0.05397 -0.02260 -0.00821 -0.00347
C36 1 0.717113 -0.306607 0.151807 11.00000 0.03638 0.02885 =
0.06396 -0.02544 -0.00475 -0.00016
AFIX 3
H36 3 0.793423 -0.336667 0.137817 11.00000 0.06741
AFIX 0
C37 1 0.681371 -0.203780 0.144108 11.00000 0.03454 0.02511 =
0.05715 -0.02099 -0.00182 -0.00280
C38 1 0.369547 -0.170698 0.207397 11.00000 0.03919 0.04205 =
0.08935 -0.03857 0.01045 -0.01486
AFIX 7
H38A 3 0.341097 -0.094898 0.157307 11.00000 71.00000
H38B 3 0.327977 -0.211568 0.201878 11.00000 71.00000
H38C 3 0.359187 -0.175537 0.274267 11.00000 71.00000
AFIX 0
C39 1 0.686630 -0.479371 0.190166 11.00000 0.05819 0.02697 =
0.07854 -0.03021 -0.01086 -0.00023
AFIX 7
H39A 3 0.743895 -0.526351 0.243432 11.00000 61.00000
H39B 3 0.623446 -0.507943 0.207074 11.00000 61.00000
H39C 3 0.719909 -0.478009 0.127041 11.00000 61.00000
AFIX 0
C40 1 0.764161 -0.142249 0.112807 11.00000 0.03610 0.04384 =
0.12721 -0.04705 0.00970 -0.00880
AFIX 7
H40A 3 0.758043 -0.108728 0.156041 11.00000 51.00000
H40B 3 0.841617 -0.191798 0.117705 11.00000 51.00000
H40C 3 0.749162 -0.084731 0.043045 11.00000 51.00000
AFIX 0
C41 1 0.506447 0.386854 0.014555 11.00000 0.04271 0.01962 =
0.03490 -0.01553 0.01175 -0.01058
C42 1 0.580431 0.333415 0.105306 11.00000 0.03611 0.01845 =
0.04025 -0.01763 0.01301 -0.00977
C43 1 0.688872 0.336676 0.099809 11.00000 0.03482 0.02722 =
0.05565 -0.02482 0.01898 -0.01356
AFIX 3
H43 3 0.719472 0.375256 0.037269 11.00000 0.05433
AFIX 0
C44 1 0.752060 0.283963 0.185302 11.00000 0.02956 0.03003 =
0.07738 -0.03206 0.01182 -0.01093
AFIX 3
H44 3 0.826540 0.285413 0.183072 11.00000 0.03904
AFIX 0
C45 1 0.705601 0.228160 0.275572 11.00000 0.03635 0.03013 =
0.05857 -0.02201 -0.00017 -0.01055
AFIX 3
H45 3 0.748031 0.190430 0.335792 11.00000 0.04960
AFIX 0
C46 1 0.596624 0.228342 0.277471 11.00000 0.03436 0.02424 =
0.04138 -0.01374 0.00314 -0.01047
AFIX 3
H46 3 0.565014 0.189982 0.339591 11.00000 0.04285
AFIX 0
HKLF 4
REM 09SRV337 OLEX2: imported from CIF
REM wR2 = 0.0700, GooF = S = 1.064, Restrained GooF = 1.064 for all data
REM R1 = 0.0264 for 12254 Fo > 4sig(Fo) and 0.0322 for all 13912 data
REM 533 parameters refined using 0 restraints
END
WGHT 0.0382 0.0859
REM Highest difference peak 2.497, deepest hole -0.788, 1-sigma level 0.094
Q1 1 0.3994 0.2794 0.2248 11.00000 0.05 2.50
Q2 1 0.3467 0.2993 0.1202 11.00000 0.05 1.37
Q3 1 0.3155 0.2761 0.2041 11.00000 0.05 1.19
Q4 1 0.4183 0.2996 0.1533 11.00000 0.05 1.08
Q5 1 0.5624 0.2777 0.2254 11.00000 0.05 0.54
Q6 1 0.4417 0.1032 0.2043 11.00000 0.05 0.49
Q7 1 0.2006 0.2810 0.1278 11.00000 0.05 0.47
Q8 1 0.1648 0.5766 0.1432 11.00000 0.05 0.47
Q9 1 0.5555 0.3560 0.0567 11.00000 0.05 0.46
Q10 1 0.5855 -0.0191 0.2608 11.00000 0.05 0.45
Q11 1 0.1440 0.8034 0.1032 11.00000 0.05 0.44
Q12 1 0.0554 0.7002 0.2565 11.00000 0.05 0.44
Q13 1 0.3305 0.1972 0.3582 11.00000 0.05 0.43
Q14 1 0.1366 0.5745 0.1981 11.00000 0.05 0.42
Q15 1 0.7376 0.2445 0.2197 11.00000 0.05 0.42
Q16 1 0.2228 0.4398 0.2034 11.00000 0.05 0.41
Q17 1 0.5367 -0.0586 0.2181 11.00000 0.05 0.40
;
_shelx_res_checksum 28895
_shelx_fab_file
;
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-17 -8 1 1.8070 2.4972
-17 -8 2 -1.3701 -1.9020
-17 -7 1 -0.8072 -0.8975
-17 -7 2 0.7190 0.0280
-17 -6 1 -0.5036 -2.1391
-17 -6 2 0.7765 1.9602
-17 -5 1 -1.1070 1.8257
-17 -5 2 1.1114 -0.1988
-17 -5 3 0.1158 -1.4237
-17 -4 1 0.3251 1.3287
-17 -4 2 -0.2386 -1.1444
-17 -4 3 0.5582 0.1564
-17 -3 1 0.7328 -2.2613
-17 -3 2 -1.1538 0.5506
-17 -2 1 -0.9970 -0.4935
-17 -2 2 0.0050 1.1850
-16 -11 1 -0.1374 -2.6383
-16 -11 2 0.0217 1.9887
-16 -10 1 -0.6381 0.7292
-16 -10 2 0.0220 -0.2534
-16 -10 3 0.0907 -0.9854
-16 -9 1 1.2423 1.9218
-16 -9 2 -0.1869 -1.3010
-16 -9 3 -0.2783 0.0180
-16 -8 1 0.3902 -1.4403
-16 -8 2 -0.0284 0.0830
-16 -8 3 0.2276 0.4783
-16 -8 4 -0.9940 0.0676
-16 -7 1 0.9960 -0.7274
-16 -7 2 -0.3949 -0.5161
-16 -7 3 -0.1119 0.7499
-16 -7 4 -0.2143 0.0404
-16 -7 5 0.1628 -1.1126
-16 -6 1 -0.2641 1.8107
-16 -6 2 0.8249 -0.4723
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-16 -4 1 -0.6613 -1.7130
-16 -4 2 1.6129 0.3487
-16 -4 3 -1.0059 -0.0254
-16 -4 4 -0.8429 0.4557
-16 -4 5 1.3193 -0.3448
-16 -4 6 -0.1223 -0.5470
-16 -3 1 0.5968 0.5375
-16 -3 2 -0.9921 -0.8327
-16 -3 3 0.4369 0.8238
-16 -3 4 0.0084 -0.0268
-16 -3 5 -0.1687 -1.0669
-16 -3 6 0.4741 1.5209
-16 -2 1 -0.3405 1.3532
-16 -2 2 -0.9322 -0.0245
-16 -2 3 1.9533 -0.0956
-16 -2 4 -1.3228 -0.5873
-16 -2 5 0.3114 0.7919
-16 -2 6 -0.2199 -0.0764
-16 -1 1 1.0251 -1.3598
-16 -1 2 0.5428 0.9806
-16 -1 3 -0.4114 -0.6214
-16 -1 4 0.1240 0.3732
-16 -1 5 -0.3043 0.4435
-16 -1 6 0.3395 -1.7726
-16 0 1 0.2272 -1.1991
-16 0 2 0.2475 0.6780
-16 0 3 0.1778 0.2706
-16 0 4 -0.5634 -0.0251
-16 0 5 0.6417 -1.3912
-16 1 1 -0.4874 2.2331
-16 1 2 -0.1160 -0.7741
-16 1 3 0.8456 -0.2843
-16 1 4 -0.5186 -0.2022
-16 2 1 -0.2357 0.4957
-16 2 2 0.5535 -0.9135
-15 -13 1 -0.1997 -1.8654
-15 -12 1 1.1823 -2.0104
-15 -12 2 -1.0123 1.8358
-15 -11 1 -2.3108 2.0941
-15 -11 2 1.2195 -0.5827
-15 -11 3 0.3277 -1.3624
-15 -10 1 -0.5346 0.3143
-15 -10 2 0.0198 0.2692
-15 -10 3 0.3063 -1.0300
-15 -10 4 -0.5062 1.4687
-15 -9 1 0.6882 -2.1752
-15 -9 2 0.2829 0.6832
-15 -9 3 -0.6706 0.1045
-15 -9 4 0.1458 0.4227
-15 -9 5 0.1434 -1.3373
-15 -8 1 0.8702 0.3568
-15 -8 2 -0.0185 -1.0521
-15 -8 3 -1.2817 0.7109
-15 -8 4 1.0525 0.3423
-15 -8 5 -0.2524 -1.1131
-15 -8 6 0.3214 1.2583
-15 -7 1 0.7388 1.6672
-15 -7 2 -0.8684 -0.7683
-15 -7 3 0.1181 0.2533
-15 -7 4 -0.3311 -0.0907
-15 -7 5 0.9994 -0.1638
-15 -7 6 -0.6909 0.7492
-15 -6 1 0.8752 -1.6113
-15 -6 2 0.1257 1.5014
-15 -6 3 -1.3056 -0.6075
-15 -6 4 0.8280 -0.3553
-15 -6 5 0.4912 0.6683
-15 -6 6 -0.8383 0.1157
-15 -6 7 0.8248 -1.2564
-15 -5 1 1.0816 -1.2494
-15 -5 2 -0.4508 0.1375
-15 -5 3 -0.9184 0.1111
-15 -5 4 0.7499 0.2874
-15 -5 5 0.4349 -0.1549
-15 -5 6 -0.6678 -0.7745
-15 -5 7 0.5907 1.5694
-15 -4 1 -0.2288 2.2382
-15 -4 2 0.3726 -1.8069
-15 -4 3 -0.8457 0.6197
-15 -4 4 0.1817 0.3690
-15 -4 5 0.7322 -0.4516
-15 -4 6 -0.1365 -0.1700
-15 -4 7 -0.6942 0.8068
-15 -4 8 0.5431 -1.0137
-15 -3 1 -0.1379 0.2749
-15 -3 2 0.6054 0.4561
-15 -3 3 -1.0257 -0.1976
-15 -3 4 0.1538 -0.2225
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15 4 11 -0.8211 0.1085
15 5 0 -0.0512 -2.1689
15 5 1 -1.0550 2.0594
15 5 2 0.4441 -0.9786
15 5 3 0.3166 -0.1457
15 5 4 0.3090 0.3355
15 5 5 -0.4638 0.0814
15 5 6 0.2768 -0.0068
15 5 7 -0.8229 -0.5372
15 5 8 0.6237 0.6187
15 5 9 0.2515 -0.1145
15 5 10 -0.1929 -0.3098
15 5 11 -0.3521 0.3439
15 5 12 0.2826 -0.2266
15 6 0 -0.8366 -0.7325
15 6 1 0.3381 -0.0616
15 6 2 -0.2731 -0.0126
15 6 3 -0.0550 0.4496
15 6 4 1.1738 -0.6408
15 6 5 -1.1720 0.5220
15 6 6 0.4167 -0.2505
15 6 7 -0.8816 -0.0405
15 6 8 1.5529 0.2844
15 6 9 -1.1527 -0.4875
15 6 10 0.4575 0.6066
15 6 11 -0.1888 -0.4455
15 6 12 0.0085 -0.0147
15 6 13 -0.0672 0.3992
15 7 0 0.3630 2.4672
15 7 1 -1.0517 -2.1300
15 7 2 0.4917 0.8385
15 7 3 0.1758 -0.0177
15 7 4 0.4446 0.0796
15 7 5 -0.8547 -0.2394
15 7 6 0.3840 -0.0705
15 7 7 -0.5126 0.5801
15 7 8 1.1335 -0.7170
15 7 9 -1.1226 0.3332
15 7 10 0.6682 0.2628
15 7 11 -0.5542 -0.6072
15 7 12 0.1856 0.6018
15 7 13 0.3999 -0.6541
15 8 0 -0.4599 -0.3333
15 8 1 -0.0610 0.5417
15 8 2 -0.4668 -0.3381
15 8 3 1.2964 -0.2626
15 8 4 -0.8045 0.6942
15 8 5 0.2633 -0.5511
15 8 6 -1.0207 0.2378
15 8 7 1.5941 -0.1927
15 8 8 -0.8163 0.1900
15 8 9 -0.2174 0.1423
15 8 10 0.2872 -0.4390
15 8 11 -0.0537 0.2689
15 8 12 -0.4402 0.0802
15 8 13 1.1353 -0.3644
15 8 14 -0.3984 0.4999
15 9 0 -1.4645 -2.5020
15 9 1 1.4149 1.5627
15 9 2 -0.9369 -0.6755
15 9 3 0.7640 0.3333
15 9 4 -0.4931 -0.3240
15 9 5 0.6247 0.3062
15 9 6 -1.4732 -0.0718
15 9 7 1.6827 -0.2968
15 9 8 -0.7754 0.4813
15 9 9 0.3310 -0.2341
15 9 10 -1.0246 -0.0752
15 9 11 0.4663 0.1071
15 9 12 1.0464 -0.2290
15 9 13 -0.3514 0.3559
15 9 14 -1.0892 -0.0471
15 10 0 1.0662 1.0676
15 10 1 -1.3888 -1.5064
15 10 2 0.8165 0.8235
15 10 3 0.7409 0.3158
15 10 4 -1.3473 -0.7197
15 10 5 0.5707 0.3324
15 10 6 0.1202 -0.0914
15 10 7 -0.2605 0.2475
15 10 8 0.2556 -0.1760
15 10 9 0.5598 -0.1126
15 10 10 -2.9351 0.2518
15 10 11 3.7789 -0.3616
15 10 12 -1.5085 0.2604
15 10 13 0.1031 0.2590
15 10 14 -0.3947 -0.6415
15 11 0 1.7322 1.9951
15 11 1 -0.5241 -1.0757
15 11 2 0.0001 0.4497
15 11 3 -0.0232 -0.3099
15 11 4 0.6589 0.3777
15 11 5 -1.2603 -0.5343
15 11 6 0.9923 0.2727
15 11 7 -0.3555 0.4930
15 11 8 0.3675 -0.7409
15 11 9 -0.6998 0.2242
15 11 10 -0.7482 0.0577
15 11 11 2.6521 0.0620
15 11 12 -2.3099 0.0482
15 11 13 2.0204 -0.3105
15 11 14 -2.6913 0.4361
15 12 0 -1.2344 -2.0849
15 12 1 0.5780 1.8213
15 12 2 0.5185 -0.7113
15 12 3 -0.8710 -0.2945
15 12 4 0.8329 0.1267
15 12 5 -0.8072 0.1964
15 12 6 0.7260 0.2420
15 12 7 -0.6501 -0.6675
15 12 8 0.5570 0.5129
15 12 9 -0.7330 -0.1201
15 12 10 0.0746 -0.3247
15 12 11 1.0382 0.5613
15 12 12 -0.2778 -0.1745
15 12 13 -0.6644 -0.3066
15 12 14 0.1689 0.4132
15 13 0 0.2419 -1.3533
15 13 1 -0.3079 0.8812
15 13 2 0.6808 -0.3222
15 13 3 -0.7598 0.0081
15 13 4 0.7074 -0.5287
15 13 5 -0.4738 0.7526
15 13 6 0.3745 -0.0134
15 13 7 -1.0045 -0.4120
15 13 8 1.3529 0.0130
15 13 9 -1.0579 -0.0195
15 13 10 0.0373 0.6282
15 13 11 1.1977 -0.6310
15 13 12 -0.6537 0.0761
15 13 13 -0.3832 0.3998
15 13 14 -0.0165 -0.6935
15 14 0 -0.6279 1.8981
15 14 1 0.0068 -1.2700
15 14 2 -0.0231 0.5401
15 14 3 1.1109 -0.7378
15 14 4 -1.3259 0.5006
15 14 5 0.3509 0.2710
15 14 6 0.4291 -0.3010
15 14 7 -0.8525 -0.1320
15 14 8 0.7227 -0.1910
15 14 9 -0.7242 0.6980
15 14 10 1.1693 -0.2259
15 14 11 -1.0163 -0.3961
15 14 12 1.0029 0.4229
15 14 13 -1.1749 -0.1209
15 14 14 0.5557 -0.2901
15 15 2 -0.4055 -1.7438
15 15 3 0.9832 -0.0522
15 15 4 -1.6983 1.2844
15 15 5 1.9109 -0.6876
15 15 6 -1.7776 -0.2470
15 15 7 0.9415 0.1435
15 15 8 -0.4190 0.1556
15 15 9 0.4471 0.1630
15 15 10 0.1138 -0.3726
15 15 11 -0.6983 0.4642
15 15 12 1.0444 -0.4119
15 15 13 -1.1111 -0.1030
15 16 4 0.6776 0.6007
15 16 5 -0.9183 -0.4250
15 16 6 0.4566 0.0211
15 16 7 -0.2019 -0.3330
15 16 8 0.0890 0.4731
15 16 9 0.5641 0.1717
15 16 10 -1.0913 -0.1502
15 16 11 1.6589 -0.3547
15 16 12 -2.0806 0.2515
15 17 8 0.2431 0.9461
15 17 9 0.9258 -1.1378
16 -2 0 -1.0302 0.9895
16 -1 0 0.3949 2.1331
16 -1 1 -0.8696 -0.5877
16 -1 2 0.9856 -0.5600
16 -1 3 -0.3250 0.3598
16 0 0 -0.6750 -0.9299
16 0 1 -0.5114 0.7036
16 0 2 0.9616 -0.6560
16 0 3 0.4786 0.1189
16 0 4 -0.8613 0.6931
16 0 5 0.0739 -0.9484
16 1 0 -2.9276 -1.2265
16 1 1 2.0760 0.5486
16 1 2 -0.2635 -0.0653
16 1 3 0.0462 0.1725
16 1 4 0.0281 -0.3857
16 1 5 -0.1415 0.1034
16 1 6 -0.2319 0.6505
16 2 0 0.3470 2.4387
16 2 1 -0.3449 -1.9978
16 2 2 0.3339 0.6315
16 2 3 0.3118 0.1427
16 2 4 -0.4708 0.0123
16 2 5 0.6610 -0.1444
16 2 6 -0.9419 -0.1747
16 2 7 -0.0439 0.7033
16 3 0 0.6454 0.3544
16 3 1 -1.6865 -0.1741
16 3 2 0.9422 -0.0578
16 3 3 0.7296 -0.0350
16 3 4 -0.6169 0.5622
16 3 5 0.0936 -0.8966
16 3 6 -0.8623 0.6872
16 3 7 1.1293 -0.1370
16 3 8 -0.5137 -0.4658
16 3 9 -0.0725 0.7731
16 4 0 -0.0850 -2.7049
16 4 1 -0.5003 2.1341
16 4 2 0.8182 -0.7146
16 4 3 0.1536 -0.0264
16 4 4 -0.5117 -0.1729
16 4 5 0.3440 0.3055
16 4 6 -0.6185 0.2978
16 4 7 0.4942 -0.9711
16 4 8 -0.5196 0.8728
16 4 9 1.0418 -0.4508
16 5 0 -0.1384 0.5859
16 5 1 -1.2187 -0.6238
16 5 2 2.0918 0.2905
16 5 3 -1.1977 0.0827
16 5 4 0.2932 -0.4136
16 5 5 0.1841 0.5670
16 5 6 -0.6689 -0.2035
16 5 7 0.1735 -0.3729
16 5 8 0.3357 0.3564
16 5 9 0.3294 0.0405
16 5 10 -0.6859 0.0100
16 6 0 0.2242 2.4562
16 6 1 -0.7096 -1.8357
16 6 2 0.6810 0.5796
16 6 3 0.1644 -0.0697
16 6 4 -0.1009 0.4168
16 6 5 -0.6881 -0.4419
16 6 6 0.5805 -0.1011
16 6 7 -0.2947 0.2670
16 6 8 0.3827 0.1410
16 6 9 -0.3904 -0.2754
16 6 10 0.7484 -0.1766
16 6 11 -1.4821 0.5930
16 7 0 -0.6995 -1.5749
16 7 1 0.0799 1.2550
16 7 2 0.0489 -0.5418
16 7 3 0.3437 -0.0024
16 7 4 0.1503 0.3544
16 7 5 -1.2399 -0.4201
16 7 6 1.1042 0.2225
16 7 7 -0.3934 -0.0493
16 7 8 0.3388 0.0899
16 7 9 -0.3613 -0.2003
16 7 10 -0.1905 0.2706
16 7 11 0.6348 -0.3473
16 8 0 -0.4587 -1.8809
16 8 1 0.2872 0.9273
16 8 2 -0.1284 -0.1550
16 8 3 0.4087 0.3222
16 8 4 -0.3664 -0.7175
16 8 5 -0.3822 0.6251
16 8 6 0.6598 -0.0751
16 8 7 -0.4906 -0.3498
16 8 8 0.7802 0.3412
16 8 9 -1.2751 -0.1743
16 8 10 1.0355 0.2629
16 8 11 -0.5715 -0.5781
16 8 12 0.4939 0.6075
16 9 0 -1.3774 1.9237
16 9 1 0.4141 -1.6282
16 9 2 0.7116 0.7739
16 9 3 -0.5093 0.0912
16 9 4 -0.4756 -0.2990
16 9 5 0.6729 0.1516
16 9 6 -0.3724 -0.1206
16 9 7 0.1207 0.2799
16 9 8 0.3385 -0.4443
16 9 9 -0.9116 0.4571
16 9 10 0.7579 -0.2247
16 9 11 -0.5606 -0.2034
16 9 12 1.1910 0.3831
16 10 0 1.2132 0.3991
16 10 1 -0.9358 -0.1718
16 10 2 0.2458 0.1221
16 10 3 0.6065 -0.3427
16 10 4 -1.1441 0.7584
16 10 5 1.0565 -0.6987
16 10 6 -1.3883 0.0907
16 10 7 2.2126 0.2642
16 10 8 -2.2642 0.0452
16 10 9 1.5211 -0.2483
16 10 10 -1.9608 -0.3013
16 10 11 2.9901 0.8805
16 10 12 -1.6325 -0.8434
16 11 0 -0.0916 -2.7099
16 11 1 0.5134 1.5427
16 11 2 -0.4181 -0.2628
16 11 3 0.3207 -0.0017
16 11 4 -0.3612 -0.2736
16 11 5 -0.1715 0.1060
16 11 6 0.6080 0.3758
16 11 7 -0.3705 -0.3426
16 11 8 0.3188 -0.0007
16 11 9 -1.0219 -0.0499
16 11 10 0.4387 0.2396
16 11 11 2.0313 -0.2011
16 11 12 -2.5577 0.1506
16 12 0 2.0107 0.7788
16 12 1 -1.5618 -0.8124
16 12 2 1.2478 0.5839
16 12 3 -1.2514 -0.0722
16 12 4 1.2163 -0.7452
16 12 5 -1.4611 1.0157
16 12 6 1.4727 -0.2002
16 12 7 -0.6904 -0.5007
16 12 8 -0.4685 0.1957
16 12 9 0.6551 0.1964
16 12 10 -0.2957 0.0909
16 12 11 1.0506 -0.5734
16 12 12 -1.2441 0.8333
16 13 1 1.3934 -0.1508
16 13 2 -1.0277 0.3412
16 13 3 0.2828 -0.7364
16 13 4 0.1146 0.6606
16 13 5 -0.3504 0.0011
16 13 6 0.4724 -0.2383
16 13 7 -0.8211 0.0293
16 13 8 1.2271 -0.0754
16 13 9 -1.4673 0.2203
16 13 10 1.2967 -0.2116
16 13 11 0.2050 0.5078
16 13 12 -1.3125 -0.7960
16 14 2 -0.0217 -1.6242
16 14 3 -0.1878 0.3503
16 14 4 0.2126 0.6939
16 14 5 -0.2901 -0.3537
16 14 6 -0.1833 -0.0069
16 14 7 0.7555 -0.3401
16 14 8 -0.8058 0.3213
16 14 9 0.4420 0.1732
16 14 10 0.2820 0.1042
16 14 11 -0.1789 -0.8092
16 15 5 1.0375 -0.7074
16 15 6 -0.1909 -0.0878
16 15 7 -0.5802 -0.0619
16 15 8 0.4883 0.5644
16 15 9 0.6272 -0.0217
16 15 10 -1.0020 -0.7838
17 2 0 0.3916 -0.0712
17 2 1 0.3542 0.3178
17 2 2 0.4313 -0.6044
17 2 3 -0.7629 0.2491
17 2 4 0.1143 0.5552
17 3 0 -0.1585 -2.1195
17 3 1 0.0920 0.7782
17 3 2 -0.1532 -0.0422
17 3 3 0.5954 0.3567
17 3 4 -0.6211 -0.5042
17 3 5 -0.0307 -0.0344
17 4 0 -0.4449 1.0722
17 4 1 0.2370 -1.0437
17 4 2 0.0468 0.9380
17 4 3 0.5571 -0.1797
17 4 4 -1.0225 -0.6023
17 4 5 0.3688 0.4997
17 4 6 -0.1155 0.1670
17 5 0 0.5198 1.6772
17 5 1 -0.6982 -0.4069
17 5 2 1.7665 -0.1436
17 5 3 -1.9313 -0.3885
17 5 4 0.8614 0.8205
17 5 5 0.0933 -0.4883
17 5 6 -0.6068 0.0800
17 5 7 0.3576 -0.2560
17 6 0 0.0367 -1.8183
17 6 1 0.0049 1.3178
17 6 2 0.6020 -0.8287
17 6 3 -1.0226 0.2699
17 6 4 0.8407 0.2064
17 6 5 -0.4117 -0.1891
17 6 6 -0.4706 -0.0191
17 6 7 0.9725 -0.3707
17 6 8 -0.3596 1.0490
17 7 0 0.9272 -0.8310
17 7 1 -0.8008 -0.0499
17 7 2 0.3353 0.3259
17 7 3 0.2472 0.3833
17 7 4 -0.3148 -0.8634
17 7 5 -0.6494 0.5660
17 7 6 1.3584 -0.1834
17 7 7 -0.8844 0.0676
17 7 8 -0.1111 0.2087
17 7 9 0.8467 -0.6882
17 8 0 -1.3393 1.8989
17 8 1 0.2569 -1.2542
17 8 2 0.6019 0.8434
17 8 3 -0.5620 -0.3643
17 8 4 -0.2385 0.0539
17 8 5 0.3638 -0.0283
17 8 6 0.4089 -0.0257
17 8 7 -1.1170 0.3090
17 8 8 1.2858 -0.5382
17 8 9 -1.0463 0.4090
17 9 0 -0.3041 -0.0679
17 9 1 0.6549 0.6955
17 9 2 -0.7850 -0.3640
17 9 3 0.7564 -0.3175
17 9 4 -1.0859 0.7102
17 9 5 1.2386 -0.5093
17 9 6 -1.0181 0.1162
17 9 7 1.0129 -0.0418
17 9 8 -1.1988 0.1026
17 9 9 0.8169 0.0504
17 9 10 0.0064 -0.2688
17 10 0 -0.3126 -0.9317
17 10 1 0.1813 0.7850
17 10 2 -0.0073 -0.4952
17 10 3 -0.4794 0.5347
17 10 4 0.4930 -0.4510
17 10 5 -0.0995 0.1561
17 10 6 -0.1104 0.1014
17 10 7 -0.1084 -0.3650
17 10 8 0.7703 0.4793
17 10 9 -1.5889 -0.0760
17 10 10 1.5433 -0.6291
17 11 1 -1.3842 -0.1542
17 11 2 1.6379 0.4334
17 11 3 -1.4380 0.1232
17 11 4 0.6146 -0.6255
17 11 5 0.1405 0.4308
17 11 6 -0.5961 -0.1980
17 11 7 1.3074 0.3635
17 11 8 -1.9487 -0.2727
17 11 9 1.4695 -0.5177
17 12 3 1.3565 -1.5404
17 12 4 -1.1645 0.8961
17 12 5 0.3157 -0.1229
17 12 6 0.7961 0.0511
17 12 7 -0.9699 -0.0711
17 12 8 0.0181 -0.5998
17 12 9 0.6268 1.2841
17 13 5 -0.1575 -0.1519
17 13 6 -0.0348 -0.0371
17 13 7 0.0633 -0.6466
17 13 8 -0.0115 1.2873
0 0 0 0.0 0.0
;
_shelx_fab_checksum 88312
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
#===END
_exptl_crystal_preparation Luminescent
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_3_19s248
_database_code_depnum_ccdc_archive 'CCDC 1962579'
loop_
_audit_author_name
_audit_author_address
'Andrei S. Batsanov'
;Durham University
United Kingdom
;
_audit_update_record
;
2019-11-14 deposited with the CCDC. 2020-01-23 downloaded from the CCDC.
;
_audit_creation_date 2019-11-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_shelx_SHELXL_version_number 2018/3
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C48 H34 F4 Ir N5 O2, 4(C Cl3 D)'
_chemical_formula_sum 'C52 H34 Cl12 D4 F4 Ir N5 O2'
_chemical_formula_weight 1462.50
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.0759(5)
_cell_length_b 16.3073(8)
_cell_length_c 17.9412(8)
_cell_angle_alpha 89.3872(15)
_cell_angle_beta 76.7980(14)
_cell_angle_gamma 89.1792(15)
_cell_volume 2869.6(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9895
_cell_measurement_temperature 120
_cell_measurement_theta_max 26.639
_cell_measurement_theta_min 2.410
_shelx_estimated_absorpt_T_max 0.846
_shelx_estimated_absorpt_T_min 0.765
_exptl_absorpt_coefficient_mu 2.943
_exptl_absorpt_correction_T_max 0.8948
_exptl_absorpt_correction_T_min 0.8070
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
wR2(int) was 0.0591 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9019.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.693
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1436
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 1.00 0.00 0.0390
-1.00 -1.00 0.00 0.0210
1.00 -1.00 1.00 0.0360
0.00 1.00 1.00 0.0230
0.00 -1.00 -1.00 0.0440
-1.00 0.00 1.00 0.0260
-1.00 -1.00 1.00 0.0260
1.00 0.00 -1.00 0.0480
1.00 -1.00 -1.00 0.0340
0.00 1.00 0.00 0.0370
-1.00 -1.00 -1.00 0.0220
0.00 -1.00 0.00 0.0370
0.00 0.00 -1.00 0.0510
0.00 -1.00 2.00 0.0380
-1.00 2.00 -2.00 0.0420
_exptl_crystal_size_max 0.096
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.059
_exptl_special_details
;
Data were collected in shutterless mode. Full sphere of reciprocal
space was nominally covered by 4 runs of 340 narrow-frame \w-scans (scan
width 0.5\%, 30s exposure), every run at a different \f angle.
Crystal to detector distance 3.49 cm.
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0585
_diffrn_reflns_av_unetI/netI 0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 59027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 28.500
_diffrn_reflns_theta_max 29.130
_diffrn_reflns_theta_min 2.076
_diffrn_ambient_temperature 120
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '3-circle area detector diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method \w-scan
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe X-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 1.0
_diffrn_source_power 0.05
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_source_voltage 50.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 12529
_reflns_number_total 15449
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction 'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL 2018/3 multi-CPU (Sheldrick, 2015a)'
_computing_structure_solution 'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max 2.192
_refine_diff_density_min -1.365
_refine_diff_density_rms 0.133
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.983
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 701
_refine_ls_number_reflns 15449
_refine_ls_number_restraints 52
_refine_ls_R_factor_all 0.0547
_refine_ls_R_factor_gt 0.0361
_refine_ls_restrained_S_all 0.982
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0730
_refine_ls_wR_factor_ref 0.0774
_refine_special_details
;
Mesityl group at C(15) is disordered by a ca. 11\% libration
between two orientations (A and B), with occupancies 0.542(15) and
0.458(15), respectively.
Methyl group C(47)H~3~ is ideally disordered.
Methyl groups C(46)H~3~ and C(48)H~3~ were refined as rigid (rotating)
bodies with a common (refined) U(iso) for three hydrogens. Other H
atoms - riding model (constr).
;
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
3. Same fragment restrains
{C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B} sigma for 1-2: 0.02,
1-3: 0.04
as in
{C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A}
4. Others
Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(1)
Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(2)
Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=
Sof(C17A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=
Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(3)
Sof(C12B)=Sof(C13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(C16B)=Sof(H16B)=
Sof(C17B)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19B)=Sof(H19A)=
Sof(H19B)=Sof(H19C)=Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
Fixed Sof: H39A(0.5) H39B(0.5) H39C(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
5.a Riding coordinates:
C18B(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C20B(H20A,H20B,H20C), C18A(H18D,
H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F)
5.b Ternary CH refined with riding coordinates:
C50(D50), C51(D51), C49(D49), C52(D52)
5.c Aromatic/amide H refined with riding coordinates:
C2(H2), C8(H8), C10(H10), C11(H11), C22(H22), C28(H28), C30(H30), C31(H31),
C34(H34), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46), C14B(H14B),
C16B(H16B), C14A(H14A), C16A(H16A)
5.d Disordered Me refined with riding coordinates:
C39(H39A,H39B,H39C,H39D,H39E,H39F)
5.e Idealised Me refined as rotating group:
C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir Ir 0.18605(2) 0.26604(2) 0.45391(2) 0.01078(4) Uani 1 1 d . . . . .
F1 F 0.69952(18) 0.14357(12) 0.41500(11) 0.0224(4) Uani 1 1 d . . . . .
F2 F 0.58481(19) 0.27835(12) 0.20762(10) 0.0226(4) Uani 1 1 d . . . . .
F3 F 0.0645(2) 0.03224(12) 0.27104(10) 0.0257(5) Uani 1 1 d . . . . .
F4 F 0.17598(19) -0.05212(11) 0.49813(10) 0.0179(4) Uani 1 1 d . . . . .
O1 O 0.2108(2) 0.38307(13) 0.50237(12) 0.0150(5) Uani 1 1 d . . . . .
O2 O 0.0974(2) 0.48412(14) 0.57355(14) 0.0247(5) Uani 1 1 d . . . . .
N1 N 0.1924(3) 0.32633(15) 0.35257(14) 0.0121(5) Uani 1 1 d . . . . .
N2 N 0.2025(3) 0.20125(15) 0.54888(14) 0.0122(5) Uani 1 1 d . . . . .
N3 N -0.0173(3) 0.30184(16) 0.50545(14) 0.0142(5) Uani 1 1 d . . . . .
N4 N 0.8888(3) 0.1882(2) 0.23013(18) 0.0322(8) Uani 1 1 d . . . . .
N5 N 0.1099(3) -0.16342(17) 0.34775(15) 0.0219(6) Uani 1 1 d . . . . .
C1 C 0.3797(3) 0.24218(18) 0.40170(17) 0.0121(6) Uani 1 1 d . . . . .
C2 C 0.4779(3) 0.19892(19) 0.43078(17) 0.0149(6) Uani 1 1 d . . . . .
H2 H 0.455764 0.178754 0.481947 0.018 Uiso 1 1 calc R U . . .
C3 C 0.6051(3) 0.18550(19) 0.38617(18) 0.0156(7) Uani 1 1 d . . . . .
C4 C 0.6442(3) 0.21172(19) 0.31033(18) 0.0156(6) Uani 1 1 d . . . . .
C5 C 0.5457(3) 0.25415(19) 0.28156(17) 0.0147(6) Uani 1 1 d . . . . .
C6 C 0.4166(3) 0.27108(18) 0.32466(17) 0.0134(6) Uani 1 1 d . . . . .
C7 C 0.3129(3) 0.32078(18) 0.29923(17) 0.0122(6) Uani 1 1 d . . . . .
C8 C 0.3299(3) 0.36387(19) 0.23051(17) 0.0149(6) Uani 1 1 d . . . . .
H8 H 0.412647 0.357842 0.192896 0.018 Uiso 1 1 calc R U . . .
C9 C 0.2276(3) 0.41578(19) 0.21582(17) 0.0150(6) Uani 1 1 d . . . . .
C10 C 0.1065(3) 0.42095(19) 0.27158(18) 0.0177(7) Uani 1 1 d . . . . .
H10 H 0.033943 0.455500 0.263930 0.021 Uiso 1 1 calc R U . . .
C11 C 0.0928(3) 0.37525(19) 0.33822(18) 0.0153(6) Uani 1 1 d . . . . .
H11 H 0.009196 0.378651 0.375511 0.018 Uiso 1 1 calc R U . . .
C21 C 0.1503(3) 0.15436(18) 0.42040(17) 0.0116(6) Uani 1 1 d . . . . .
C22 C 0.1142(3) 0.13341(19) 0.35215(17) 0.0161(7) Uani 1 1 d . . . . .
H22 H 0.099976 0.175023 0.317234 0.019 Uiso 1 1 calc R U . . .
C23 C 0.0996(3) 0.0528(2) 0.33617(17) 0.0158(7) Uani 1 1 d . . . . .
C24 C 0.1211(3) -0.01135(18) 0.38426(17) 0.0130(6) Uani 1 1 d . . . . .
C25 C 0.1546(3) 0.01043(18) 0.45231(17) 0.0132(6) Uani 1 1 d . . . . .
C26 C 0.1677(3) 0.09089(18) 0.47233(16) 0.0116(6) Uani 1 1 d . . . . .
C27 C 0.1986(3) 0.11796(18) 0.54446(17) 0.0116(6) Uani 1 1 d . . . . .
C28 C 0.2240(3) 0.06926(19) 0.60394(16) 0.0131(6) Uani 1 1 d . . . . .
H28 H 0.222391 0.011229 0.600193 0.016 Uiso 1 1 calc R U . . .
C29 C 0.2517(3) 0.10478(19) 0.66900(17) 0.0141(6) Uani 1 1 d . . . . .
C30 C 0.2505(3) 0.1901(2) 0.67264(18) 0.0177(7) Uani 1 1 d . . . . .
H30 H 0.266644 0.216536 0.716585 0.021 Uiso 1 1 calc R U . . .
C31 C 0.2256(3) 0.23579(19) 0.61224(17) 0.0165(7) Uani 1 1 d . . . . .
H31 H 0.224774 0.293914 0.615511 0.020 Uiso 1 1 calc R U . . .
C32 C 0.2803(3) 0.05237(19) 0.73222(17) 0.0150(6) Uani 1 1 d . . . . .
C33 C 0.4016(3) 0.0062(2) 0.72086(18) 0.0175(7) Uani 1 1 d . . . . .
C34 C 0.4252(4) -0.0431(2) 0.7805(2) 0.0242(8) Uani 1 1 d . . . . .
H34 H 0.508090 -0.073630 0.773193 0.029 Uiso 1 1 calc R U . . .
C35 C 0.3316(4) -0.0489(2) 0.84998(19) 0.0241(8) Uani 1 1 d . . . . .
C36 C 0.2140(4) -0.0018(2) 0.86052(18) 0.0218(7) Uani 1 1 d . . . . .
H36 H 0.149789 -0.004762 0.908304 0.026 Uiso 1 1 calc R U . . .
C37 C 0.1860(3) 0.05003(19) 0.80339(18) 0.0168(7) Uani 1 1 d . . . . .
C38 C 0.5080(3) 0.0109(2) 0.6469(2) 0.0244(8) Uani 1 1 d . . . . .
H38A H 0.581912 -0.028270 0.648615 0.046(7) Uiso 1 1 calc R U . . .
H38B H 0.544576 0.066524 0.639840 0.046(7) Uiso 1 1 calc R U . . .
H38C H 0.466705 -0.002485 0.604189 0.046(7) Uiso 1 1 calc R U . . .
C39 C 0.3570(5) -0.1054(3) 0.9124(2) 0.0415(11) Uani 1 1 d . . . . .
H39A H 0.444881 -0.133683 0.894923 0.062 Uiso 0.5 1 calc R U P . .
H39B H 0.358454 -0.073320 0.958117 0.062 Uiso 0.5 1 calc R U P . .
H39C H 0.284125 -0.145861 0.924854 0.062 Uiso 0.5 1 calc R U P . .
H39D H 0.280093 -0.101560 0.957006 0.062 Uiso 0.5 1 calc R U P . .
H39E H 0.366519 -0.161923 0.893813 0.062 Uiso 0.5 1 calc R U P . .
H39F H 0.440849 -0.089382 0.927076 0.062 Uiso 0.5 1 calc R U P . .
C40 C 0.0587(3) 0.1023(2) 0.81994(19) 0.0213(7) Uani 1 1 d . . . . .
H40A H 0.081016 0.157920 0.832772 0.033(6) Uiso 1 1 calc R U . . .
H40B H -0.007646 0.078669 0.863160 0.033(6) Uiso 1 1 calc R U . . .
H40C H 0.019611 0.104375 0.774679 0.033(6) Uiso 1 1 calc R U . . .
C41 C 0.1021(3) 0.4179(2) 0.54048(18) 0.0168(7) Uani 1 1 d . . . . .
C42 C -0.0297(3) 0.37379(19) 0.54355(18) 0.0162(7) Uani 1 1 d . . . . .
C43 C -0.1546(4) 0.4042(2) 0.5811(2) 0.0277(8) Uani 1 1 d . . . . .
H43 H -0.160906 0.454151 0.608574 0.033 Uiso 1 1 calc R U . . .
C44 C -0.2709(4) 0.3617(2) 0.5785(2) 0.0313(9) Uani 1 1 d . . . . .
H44 H -0.358250 0.382082 0.603752 0.038 Uiso 1 1 calc R U . . .
C45 C -0.2581(3) 0.2896(2) 0.5389(2) 0.0263(8) Uani 1 1 d . . . . .
H45 H -0.336784 0.259355 0.536343 0.032 Uiso 1 1 calc R U . . .
C46 C -0.1309(3) 0.2612(2) 0.50296(19) 0.0190(7) Uani 1 1 d . . . . .
H46 H -0.123170 0.211182 0.475486 0.023 Uiso 1 1 calc R U . . .
C47 C 0.7798(4) 0.1981(2) 0.26518(19) 0.0219(7) Uani 1 1 d . . . . .
C48 C 0.1138(3) -0.0962(2) 0.36395(17) 0.0151(6) Uani 1 1 d . . . . .
C12B C 0.2426(9) 0.4578(6) 0.1416(5) 0.012(2) Uiso 0.458(15) 1 d D U P A 1
C13B C 0.1616(10) 0.4406(6) 0.0896(4) 0.017(2) Uiso 0.458(15) 1 d D U P A 1
C14B C 0.1890(10) 0.4819(6) 0.0199(4) 0.017(2) Uiso 0.458(15) 1 d D U P A 1
H14B H 0.136222 0.470100 -0.016179 0.020 Uiso 0.458(15) 1 calc R U P A 1
C15B C 0.2896(14) 0.5393(9) 0.0013(6) 0.024(3) Uani 0.458(15) 1 d D U P A 1
C16B C 0.3684(8) 0.5576(6) 0.0525(5) 0.020(2) Uiso 0.458(15) 1 d D U P A 1
H16B H 0.437129 0.597940 0.039716 0.023 Uiso 0.458(15) 1 calc R U P A 1
C17B C 0.3467(8) 0.5163(6) 0.1239(5) 0.017(2) Uiso 0.458(15) 1 d D U P A 1
C18B C 0.0462(10) 0.3821(5) 0.1089(6) 0.022(2) Uiso 0.458(15) 1 d D U P A 1
H18A H 0.025104 0.362849 0.061380 0.033 Uiso 0.458(15) 1 d R U P A 1
H18B H -0.034286 0.409599 0.140170 0.033 Uiso 0.458(15) 1 d R U P A 1
H18C H 0.072154 0.335279 0.137360 0.033 Uiso 0.458(15) 1 d R U P A 1
C19B C 0.3160(17) 0.5848(11) -0.0755(7) 0.046(4) Uani 0.458(15) 1 d D U P A 1
H19A H 0.401277 0.615118 -0.082586 0.069 Uiso 0.458(15) 1 d R U P A 1
H19B H 0.240537 0.623288 -0.075936 0.069 Uiso 0.458(15) 1 d R U P A 1
H19C H 0.323107 0.545398 -0.117136 0.069 Uiso 0.458(15) 1 d R U P A 1
C20B C 0.4301(9) 0.5418(6) 0.1796(6) 0.024(2) Uiso 0.458(15) 1 d D U P A 1
H20A H 0.495031 0.583986 0.156158 0.036 Uiso 0.458(15) 1 d R U P A 1
H20B H 0.479821 0.493996 0.193358 0.036 Uiso 0.458(15) 1 d R U P A 1
H20C H 0.368981 0.563756 0.225798 0.036 Uiso 0.458(15) 1 d R U P A 1
C12A C 0.2612(8) 0.4701(5) 0.1454(4) 0.013(2) Uiso 0.542(15) 1 d D U P A 2
C13A C 0.1962(9) 0.4537(5) 0.0855(4) 0.0198(19) Uiso 0.542(15) 1 d D U P A 2
C14A C 0.2288(10) 0.5029(5) 0.0190(4) 0.0210(18) Uiso 0.542(15) 1 d D U P A 2
H14A H 0.185196 0.493467 -0.021721 0.025 Uiso 0.542(15) 1 calc R U P A 2
C15A C 0.3222(13) 0.5641(7) 0.0121(5) 0.024(2) Uani 0.542(15) 1 d D U P A 2
C16A C 0.3835(7) 0.5799(5) 0.0719(5) 0.0237(19) Uiso 0.542(15) 1 d D U P A 2
H16A H 0.447083 0.623215 0.066897 0.028 Uiso 0.542(15) 1 calc R U P A 2
C17A C 0.3540(7) 0.5337(5) 0.1396(4) 0.0169(18) Uiso 0.542(15) 1 d D U P A 2
C18A C 0.0939(10) 0.3857(5) 0.0894(5) 0.032(2) Uiso 0.542(15) 1 d D U P A 2
H18D H 0.082730 0.374522 0.037613 0.049 Uiso 0.542(15) 1 d R U P A 2
H18E H 0.005920 0.402282 0.121913 0.049 Uiso 0.542(15) 1 d R U P A 2
H18F H 0.127510 0.336082 0.110713 0.049 Uiso 0.542(15) 1 d R U P A 2
C19A C 0.3527(15) 0.6178(9) -0.0607(7) 0.050(4) Uani 0.542(15) 1 d D U P A 2
H19D H 0.440375 0.644898 -0.065046 0.075 Uiso 0.542(15) 1 d R U P A 2
H19E H 0.280405 0.659348 -0.057386 0.075 Uiso 0.542(15) 1 d R U P A 2
H19F H 0.356795 0.583618 -0.105746 0.075 Uiso 0.542(15) 1 d R U P A 2
C20A C 0.4163(8) 0.5552(5) 0.2044(5) 0.0235(18) Uiso 0.542(15) 1 d D U P A 2
H20D H 0.344730 0.557561 0.251583 0.035 Uiso 0.542(15) 1 d R U P A 2
H20E H 0.460260 0.608671 0.194583 0.035 Uiso 0.542(15) 1 d R U P A 2
H20F H 0.484290 0.513321 0.209793 0.035 Uiso 0.542(15) 1 d R U P A 2
Cl4 Cl 0.25804(11) 0.19210(7) 0.14390(6) 0.0425(3) Uani 1 1 d . . . . .
Cl5 Cl 0.11411(14) 0.14869(8) 0.02829(6) 0.0545(3) Uani 1 1 d . . . . .
Cl6 Cl 0.26057(12) 0.02488(7) 0.09439(7) 0.0512(3) Uani 1 1 d . . . . .
C50 C 0.1640(4) 0.1162(2) 0.1111(2) 0.0304(9) Uani 1 1 d . . . . .
D50 D 0.080071 0.105415 0.151829 0.036 Uiso 1 1 calc R U . . .
Cl7 Cl 0.52790(17) 0.16312(10) 0.92987(8) 0.0782(5) Uani 1 1 d . . . . .
Cl8 Cl 0.33990(10) 0.25255(6) 0.86046(6) 0.0364(2) Uani 1 1 d . . . . .
Cl9 Cl 0.58837(13) 0.18759(9) 0.76674(7) 0.0636(4) Uani 1 1 d . . . . .
C51 C 0.4607(4) 0.1724(2) 0.8490(2) 0.0324(9) Uani 1 1 d . . . . .
D51 D 0.413476 0.120134 0.843052 0.039 Uiso 1 1 calc R U . . .
Cl1 Cl 0.26741(11) 0.58225(7) 0.69673(8) 0.0593(4) Uani 1 1 d . . . . .
Cl2 Cl 0.51811(9) 0.55430(6) 0.58296(6) 0.0343(2) Uani 1 1 d . . . . .
Cl3 Cl 0.37336(10) 0.41826(6) 0.66837(6) 0.0394(2) Uani 1 1 d . . . . .
C49 C 0.3564(4) 0.5149(2) 0.6262(2) 0.0329(9) Uani 1 1 d . . . . .
D49 D 0.302970 0.508519 0.586004 0.039 Uiso 1 1 calc R U . . .
Cl10 Cl 0.06145(14) 0.71338(7) 0.07026(6) 0.0514(3) Uani 1 1 d . . . . .
Cl11 Cl -0.10129(12) 0.59684(9) 0.17107(9) 0.0629(4) Uani 1 1 d . . . . .
Cl12 Cl 0.08560(13) 0.69718(7) 0.22714(6) 0.0503(3) Uani 1 1 d . . . . .
C52 C 0.0568(4) 0.6457(2) 0.1477(2) 0.0293(8) Uani 1 1 d . . . . .
D52 D 0.129997 0.603134 0.131978 0.035 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir 0.01345(6) 0.00833(6) 0.01052(6) 0.00360(4) -0.00281(4) -0.00049(4)
F1 0.0187(10) 0.0245(11) 0.0263(10) 0.0070(9) -0.0105(9) 0.0058(8)
F2 0.0208(10) 0.0312(11) 0.0131(9) 0.0066(8) 0.0012(8) 0.0077(9)
F3 0.0477(13) 0.0191(10) 0.0159(9) 0.0002(8) -0.0185(10) -0.0039(9)
F4 0.0302(11) 0.0104(9) 0.0161(9) 0.0050(7) -0.0118(8) 0.0003(8)
O1 0.0161(11) 0.0110(11) 0.0176(11) 0.0012(9) -0.0027(9) -0.0015(9)
O2 0.0244(13) 0.0178(12) 0.0319(14) -0.0112(11) -0.0063(11) 0.0035(10)
N1 0.0149(13) 0.0092(12) 0.0124(12) 0.0049(10) -0.0040(11) -0.0021(10)
N2 0.0140(13) 0.0128(13) 0.0095(12) 0.0000(10) -0.0020(10) -0.0009(10)
N3 0.0159(13) 0.0129(13) 0.0134(13) 0.0043(10) -0.0027(11) -0.0002(11)
N4 0.0238(17) 0.039(2) 0.0313(18) 0.0055(15) -0.0022(15) 0.0085(15)
N5 0.0291(16) 0.0190(15) 0.0171(14) -0.0002(12) -0.0045(13) 0.0000(13)
C1 0.0150(15) 0.0067(14) 0.0149(15) 0.0027(12) -0.0042(13) 0.0001(12)
C2 0.0180(16) 0.0159(16) 0.0111(14) 0.0046(12) -0.0043(13) 0.0006(13)
C3 0.0186(16) 0.0112(15) 0.0204(16) 0.0033(13) -0.0114(14) 0.0028(13)
C4 0.0151(15) 0.0130(15) 0.0185(16) 0.0009(13) -0.0036(13) 0.0009(12)
C5 0.0190(16) 0.0126(15) 0.0118(14) 0.0017(12) -0.0023(13) 0.0011(13)
C6 0.0132(15) 0.0118(15) 0.0165(15) 0.0024(12) -0.0062(13) 0.0005(12)
C7 0.0156(15) 0.0086(14) 0.0117(14) 0.0024(11) -0.0019(12) -0.0008(12)
C8 0.0181(16) 0.0147(16) 0.0120(14) 0.0018(12) -0.0038(13) 0.0018(13)
C9 0.0194(16) 0.0110(15) 0.0149(15) 0.0026(12) -0.0046(13) -0.0016(13)
C10 0.0219(17) 0.0121(15) 0.0204(16) 0.0044(13) -0.0078(14) 0.0030(13)
C11 0.0135(15) 0.0134(15) 0.0186(16) 0.0045(13) -0.0034(13) -0.0006(12)
C21 0.0093(14) 0.0130(15) 0.0122(14) 0.0006(12) -0.0020(12) 0.0018(12)
C22 0.0193(16) 0.0156(16) 0.0144(15) 0.0063(13) -0.0059(13) -0.0010(13)
C23 0.0177(16) 0.0216(17) 0.0092(14) 0.0006(13) -0.0053(13) -0.0013(13)
C24 0.0143(15) 0.0101(15) 0.0147(15) 0.0006(12) -0.0033(13) -0.0012(12)
C25 0.0143(15) 0.0120(15) 0.0135(14) 0.0064(12) -0.0042(12) 0.0008(12)
C26 0.0119(14) 0.0134(15) 0.0100(14) -0.0003(12) -0.0031(12) -0.0014(12)
C27 0.0122(14) 0.0113(14) 0.0112(14) 0.0010(12) -0.0025(12) -0.0017(12)
C28 0.0158(15) 0.0113(15) 0.0125(14) 0.0022(12) -0.0039(13) -0.0007(12)
C29 0.0136(15) 0.0145(15) 0.0142(15) 0.0013(12) -0.0034(13) 0.0004(12)
C30 0.0249(17) 0.0168(17) 0.0135(15) -0.0002(13) -0.0087(14) -0.0020(14)
C31 0.0254(17) 0.0107(15) 0.0156(15) 0.0004(12) -0.0092(14) -0.0019(13)
C32 0.0224(17) 0.0114(15) 0.0136(15) 0.0004(12) -0.0089(13) -0.0004(13)
C33 0.0216(17) 0.0175(16) 0.0149(15) -0.0009(13) -0.0071(14) -0.0005(13)
C34 0.0283(19) 0.0225(19) 0.0249(18) -0.0014(15) -0.0132(16) 0.0075(15)
C35 0.041(2) 0.0190(18) 0.0163(16) 0.0036(14) -0.0147(16) 0.0028(16)
C36 0.0313(19) 0.0201(18) 0.0132(15) 0.0004(13) -0.0033(15) -0.0027(15)
C37 0.0241(17) 0.0141(16) 0.0140(15) 0.0016(12) -0.0081(14) -0.0040(13)
C38 0.0215(18) 0.0258(19) 0.0254(18) -0.0012(15) -0.0041(16) 0.0037(15)
C39 0.068(3) 0.034(2) 0.024(2) 0.0079(18) -0.016(2) 0.017(2)
C40 0.0242(18) 0.0204(18) 0.0184(16) 0.0005(14) -0.0032(15) 0.0006(14)
C41 0.0183(16) 0.0166(16) 0.0152(15) 0.0027(13) -0.0035(13) -0.0007(13)
C42 0.0177(16) 0.0145(16) 0.0161(15) 0.0016(13) -0.0031(13) -0.0001(13)
C43 0.0258(19) 0.0234(19) 0.033(2) -0.0092(16) -0.0034(17) 0.0016(16)
C44 0.0165(18) 0.032(2) 0.041(2) -0.0065(18) 0.0016(17) 0.0029(16)
C45 0.0154(17) 0.029(2) 0.034(2) -0.0013(17) -0.0048(16) -0.0036(15)
C46 0.0215(17) 0.0160(16) 0.0208(17) 0.0034(13) -0.0073(14) -0.0041(13)
C47 0.0220(18) 0.0240(19) 0.0208(17) 0.0010(14) -0.0073(15) 0.0055(15)
C48 0.0163(16) 0.0207(17) 0.0092(14) 0.0026(13) -0.0051(13) 0.0023(13)
C15B 0.018(6) 0.036(8) 0.017(5) 0.007(5) -0.001(4) 0.004(5)
C19B 0.036(8) 0.065(11) 0.024(6) 0.029(6) 0.018(5) 0.015(7)
C15A 0.022(6) 0.027(6) 0.021(4) 0.002(4) -0.001(4) 0.008(4)
C19A 0.052(8) 0.061(9) 0.028(6) 0.030(6) 0.007(5) 0.011(6)
Cl4 0.0468(6) 0.0355(6) 0.0462(6) -0.0085(5) -0.0124(5) 0.0003(5)
Cl5 0.0821(9) 0.0572(8) 0.0263(5) 0.0065(5) -0.0168(6) -0.0055(7)
Cl6 0.0508(7) 0.0280(6) 0.0637(8) -0.0053(5) 0.0097(6) 0.0053(5)
C50 0.040(2) 0.027(2) 0.0219(18) 0.0002(16) -0.0020(17) 0.0027(17)
Cl7 0.0949(11) 0.0952(12) 0.0605(8) -0.0056(8) -0.0530(9) 0.0339(9)
Cl8 0.0372(5) 0.0363(6) 0.0378(5) 0.0018(4) -0.0131(5) -0.0005(4)
Cl9 0.0482(7) 0.0762(9) 0.0549(7) -0.0217(7) 0.0141(6) -0.0194(7)
C51 0.035(2) 0.029(2) 0.036(2) 0.0007(18) -0.0139(19) 0.0002(17)
Cl1 0.0306(6) 0.0395(6) 0.0957(10) -0.0348(7) 0.0131(6) -0.0082(5)
Cl2 0.0270(5) 0.0324(5) 0.0418(5) -0.0080(4) -0.0031(4) -0.0114(4)
Cl3 0.0270(5) 0.0325(5) 0.0555(7) -0.0031(5) -0.0024(5) -0.0069(4)
C49 0.0213(19) 0.027(2) 0.049(2) -0.0129(19) -0.0045(18) -0.0060(16)
Cl10 0.0903(9) 0.0350(6) 0.0286(5) 0.0000(4) -0.0144(6) 0.0246(6)
Cl11 0.0345(6) 0.0607(8) 0.0891(10) -0.0049(8) -0.0047(7) 0.0004(6)
Cl12 0.0727(8) 0.0484(7) 0.0376(6) -0.0100(5) -0.0296(6) 0.0164(6)
C52 0.036(2) 0.0220(19) 0.029(2) 0.0000(16) -0.0069(18) 0.0068(16)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir O1 2.147(2) . ?
Ir N1 2.046(2) . ?
Ir N2 2.033(2) . ?
Ir N3 2.123(3) . ?
Ir C1 1.996(3) . ?
Ir C21 1.987(3) . ?
F1 C3 1.356(3) . ?
F2 C5 1.351(3) . ?
F3 C23 1.343(3) . ?
F4 C25 1.349(3) . ?
O1 C41 1.280(4) . ?
O2 C41 1.233(4) . ?
N1 C7 1.366(4) . ?
N1 C11 1.342(4) . ?
N2 C27 1.363(4) . ?
N2 C31 1.342(4) . ?
N3 C42 1.354(4) . ?
N3 C46 1.341(4) . ?
N4 C47 1.144(4) . ?
N5 C48 1.141(4) . ?
C1 C2 1.399(4) . ?
C1 C6 1.424(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.363(4) . ?
C3 C4 1.392(4) . ?
C4 C5 1.392(4) . ?
C4 C47 1.437(5) . ?
C5 C6 1.379(4) . ?
C6 C7 1.464(4) . ?
C7 C8 1.390(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(4) . ?
C9 C10 1.392(4) . ?
C9 C12B 1.468(9) . ?
C9 C12A 1.512(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(4) . ?
C11 H11 0.9500 . ?
C21 C22 1.401(4) . ?
C21 C26 1.421(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.365(4) . ?
C23 C24 1.395(4) . ?
C24 C25 1.390(4) . ?
C24 C48 1.442(4) . ?
C25 C26 1.380(4) . ?
C26 C27 1.472(4) . ?
C27 C28 1.391(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.394(4) . ?
C29 C30 1.393(4) . ?
C29 C32 1.490(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.376(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.402(4) . ?
C32 C37 1.407(4) . ?
C33 C34 1.392(4) . ?
C33 C38 1.505(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.385(5) . ?
C35 C36 1.380(5) . ?
C35 C39 1.507(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.397(4) . ?
C37 C40 1.504(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 H39D 0.9800 . ?
C39 H39E 0.9800 . ?
C39 H39F 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.510(4) . ?
C42 C43 1.373(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.380(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.370(5) . ?
C45 H45 0.9500 . ?
C45 C46 1.372(5) . ?
C46 H46 0.9500 . ?
C12B C13B 1.406(10) . ?
C12B C17B 1.408(10) . ?
C13B C14B 1.387(9) . ?
C13B C18B 1.491(10) . ?
C14B H14B 0.9500 . ?
C14B C15B 1.371(11) . ?
C15B C16B 1.382(11) . ?
C15B C19B 1.529(11) . ?
C16B H16B 0.9500 . ?
C16B C17B 1.415(9) . ?
C17B C20B 1.509(10) . ?
C18B H18A 0.9801 . ?
C18B H18B 0.9799 . ?
C18B H18C 0.9799 . ?
C19B H19A 0.9799 . ?
C19B H19B 0.9800 . ?
C19B H19C 0.9800 . ?
C20B H20A 0.9801 . ?
C20B H20B 0.9800 . ?
C20B H20C 0.9800 . ?
C12A C13A 1.411(9) . ?
C12A C17A 1.393(9) . ?
C13A C14A 1.408(9) . ?
C13A C18A 1.514(10) . ?
C14A H14A 0.9500 . ?
C14A C15A 1.366(10) . ?
C15A C16A 1.383(10) . ?
C15A C19A 1.538(10) . ?
C16A H16A 0.9500 . ?
C16A C17A 1.397(8) . ?
C17A C20A 1.488(9) . ?
C18A H18D 0.9800 . ?
C18A H18E 0.9800 . ?
C18A H18F 0.9801 . ?
C19A H19D 0.9801 . ?
C19A H19E 0.9799 . ?
C19A H19F 0.9801 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
Cl4 C50 1.755(4) . ?
Cl5 C50 1.748(4) . ?
Cl6 C50 1.758(4) . ?
C50 D50 1.0000 . ?
Cl7 C51 1.740(4) . ?
Cl8 C51 1.755(4) . ?
Cl9 C51 1.740(4) . ?
C51 D51 1.0000 . ?
Cl1 C49 1.760(4) . ?
Cl2 C49 1.764(4) . ?
Cl3 C49 1.765(4) . ?
C49 D49 1.0000 . ?
Cl10 C52 1.757(4) . ?
Cl11 C52 1.753(4) . ?
Cl12 C52 1.744(4) . ?
C52 D52 1.0000 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ir O1 87.42(9) . . ?
N1 Ir N3 95.33(10) . . ?
N2 Ir O1 94.44(9) . . ?
N2 Ir N1 173.19(10) . . ?
N2 Ir N3 91.47(10) . . ?
N3 Ir O1 77.01(9) . . ?
C1 Ir O1 99.51(10) . . ?
C1 Ir N1 80.90(11) . . ?
C1 Ir N2 92.32(11) . . ?
C1 Ir N3 175.05(11) . . ?
C21 Ir O1 173.60(10) . . ?
C21 Ir N1 97.87(11) . . ?
C21 Ir N2 80.72(11) . . ?
C21 Ir N3 98.82(11) . . ?
C21 Ir C1 84.94(12) . . ?
C41 O1 Ir 116.34(19) . . ?
C7 N1 Ir 115.84(19) . . ?
C11 N1 Ir 124.9(2) . . ?
C11 N1 C7 119.0(3) . . ?
C27 N2 Ir 116.78(19) . . ?
C31 N2 Ir 123.6(2) . . ?
C31 N2 C27 119.5(3) . . ?
C42 N3 Ir 114.8(2) . . ?
C46 N3 Ir 126.6(2) . . ?
C46 N3 C42 118.5(3) . . ?
C2 C1 Ir 127.9(2) . . ?
C2 C1 C6 118.1(3) . . ?
C6 C1 Ir 114.0(2) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 H2 119.8 . . ?
F1 C3 C2 119.9(3) . . ?
F1 C3 C4 117.0(3) . . ?
C2 C3 C4 123.1(3) . . ?
C3 C4 C47 121.8(3) . . ?
C5 C4 C3 116.2(3) . . ?
C5 C4 C47 122.0(3) . . ?
F2 C5 C4 115.4(3) . . ?
F2 C5 C6 121.5(3) . . ?
C6 C5 C4 123.1(3) . . ?
C1 C6 C7 115.5(3) . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 125.3(3) . . ?
N1 C7 C6 113.5(3) . . ?
N1 C7 C8 120.0(3) . . ?
C8 C7 C6 126.4(3) . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.1(3) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C12B 121.1(4) . . ?
C8 C9 C12A 118.0(4) . . ?
C10 C9 C8 117.5(3) . . ?
C10 C9 C12B 121.2(4) . . ?
C10 C9 C12A 124.1(4) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.3 . . ?
N1 C11 C10 122.9(3) . . ?
N1 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C22 C21 Ir 127.0(2) . . ?
C22 C21 C26 118.9(3) . . ?
C26 C21 Ir 114.0(2) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 C21 119.6(3) . . ?
C23 C22 H22 120.2 . . ?
F3 C23 C22 120.0(3) . . ?
F3 C23 C24 116.8(3) . . ?
C22 C23 C24 123.2(3) . . ?
C23 C24 C48 122.3(3) . . ?
C25 C24 C23 116.6(3) . . ?
C25 C24 C48 121.1(3) . . ?
F4 C25 C24 116.1(3) . . ?
F4 C25 C26 121.1(3) . . ?
C26 C25 C24 122.8(3) . . ?
C21 C26 C27 115.7(3) . . ?
C25 C26 C21 118.9(3) . . ?
C25 C26 C27 125.4(3) . . ?
N2 C27 C26 112.2(3) . . ?
N2 C27 C28 120.1(3) . . ?
C28 C27 C26 127.7(3) . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.7(3) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 C32 120.5(3) . . ?
C30 C29 C28 117.7(3) . . ?
C30 C29 C32 121.8(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 C29 119.7(3) . . ?
C31 C30 H30 120.2 . . ?
N2 C31 C30 122.4(3) . . ?
N2 C31 H31 118.8 . . ?
C30 C31 H31 118.8 . . ?
C33 C32 C29 119.9(3) . . ?
C33 C32 C37 120.2(3) . . ?
C37 C32 C29 119.9(3) . . ?
C32 C33 C38 121.5(3) . . ?
C34 C33 C32 118.9(3) . . ?
C34 C33 C38 119.6(3) . . ?
C33 C34 H34 119.0 . . ?
C35 C34 C33 122.0(3) . . ?
C35 C34 H34 119.0 . . ?
C34 C35 C39 121.0(3) . . ?
C36 C35 C34 118.2(3) . . ?
C36 C35 C39 120.8(3) . . ?
C35 C36 H36 118.8 . . ?
C35 C36 C37 122.3(3) . . ?
C37 C36 H36 118.8 . . ?
C32 C37 C40 122.2(3) . . ?
C36 C37 C32 118.3(3) . . ?
C36 C37 C40 119.5(3) . . ?
C33 C38 H38A 109.5 . . ?
C33 C38 H38B 109.5 . . ?
C33 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39A 109.5 . . ?
C35 C39 H39B 109.5 . . ?
C35 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
H39D C39 H39E 109.5 . . ?
H39D C39 H39F 109.5 . . ?
H39E C39 H39F 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O1 C41 C42 116.4(3) . . ?
O2 C41 O1 125.2(3) . . ?
O2 C41 C42 118.4(3) . . ?
N3 C42 C41 115.3(3) . . ?
N3 C42 C43 121.6(3) . . ?
C43 C42 C41 123.0(3) . . ?
C42 C43 H43 120.3 . . ?
C42 C43 C44 119.4(3) . . ?
C44 C43 H43 120.3 . . ?
C43 C44 H44 120.6 . . ?
C45 C44 C43 118.8(3) . . ?
C45 C44 H44 120.6 . . ?
C44 C45 H45 120.2 . . ?
C44 C45 C46 119.7(3) . . ?
C46 C45 H45 120.2 . . ?
N3 C46 C45 122.0(3) . . ?
N3 C46 H46 119.0 . . ?
C45 C46 H46 119.0 . . ?
N4 C47 C4 178.7(4) . . ?
N5 C48 C24 179.1(3) . . ?
C13B C12B C9 123.2(7) . . ?
C13B C12B C17B 120.9(7) . . ?
C17B C12B C9 115.9(7) . . ?
C12B C13B C18B 121.7(7) . . ?
C14B C13B C12B 118.0(8) . . ?
C14B C13B C18B 120.3(7) . . ?
C13B C14B H14B 118.8 . . ?
C15B C14B C13B 122.3(8) . . ?
C15B C14B H14B 118.8 . . ?
C14B C15B C16B 120.2(8) . . ?
C14B C15B C19B 121.1(9) . . ?
C16B C15B C19B 118.7(9) . . ?
C15B C16B H16B 120.0 . . ?
C15B C16B C17B 120.0(8) . . ?
C17B C16B H16B 120.0 . . ?
C12B C17B C16B 118.6(8) . . ?
C12B C17B C20B 123.2(7) . . ?
C16B C17B C20B 118.0(7) . . ?
C13B C18B H18A 109.1 . . ?
C13B C18B H18B 109.8 . . ?
C13B C18B H18C 109.5 . . ?
H18A C18B H18B 109.5 . . ?
H18A C18B H18C 109.5 . . ?
H18B C18B H18C 109.5 . . ?
C15B C19B H19A 109.3 . . ?
C15B C19B H19B 109.5 . . ?
C15B C19B H19C 109.7 . . ?
H19A C19B H19B 109.5 . . ?
H19A C19B H19C 109.5 . . ?
H19B C19B H19C 109.5 . . ?
C17B C20B H20A 109.8 . . ?
C17B C20B H20B 109.4 . . ?
C17B C20B H20C 109.2 . . ?
H20A C20B H20B 109.5 . . ?
H20A C20B H20C 109.5 . . ?
H20B C20B H20C 109.5 . . ?
C13A C12A C9 117.6(6) . . ?
C17A C12A C9 121.2(6) . . ?
C17A C12A C13A 121.2(6) . . ?
C12A C13A C18A 123.1(6) . . ?
C14A C13A C12A 118.0(7) . . ?
C14A C13A C18A 118.9(7) . . ?
C13A C14A H14A 119.4 . . ?
C15A C14A C13A 121.1(7) . . ?
C15A C14A H14A 119.4 . . ?
C14A C15A C16A 119.9(7) . . ?
C14A C15A C19A 119.5(8) . . ?
C16A C15A C19A 120.5(8) . . ?
C15A C16A H16A 119.2 . . ?
C15A C16A C17A 121.5(7) . . ?
C17A C16A H16A 119.2 . . ?
C12A C17A C16A 118.2(7) . . ?
C12A C17A C20A 121.6(6) . . ?
C16A C17A C20A 120.1(6) . . ?
C13A C18A H18D 109.1 . . ?
C13A C18A H18E 110.0 . . ?
C13A C18A H18F 109.4 . . ?
H18D C18A H18E 109.5 . . ?
H18D C18A H18F 109.5 . . ?
H18E C18A H18F 109.5 . . ?
C15A C19A H19D 109.3 . . ?
C15A C19A H19E 109.4 . . ?
C15A C19A H19F 109.8 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C17A C20A H20D 109.1 . . ?
C17A C20A H20E 109.7 . . ?
C17A C20A H20F 109.6 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
Cl4 C50 Cl6 109.8(2) . . ?
Cl4 C50 D50 108.4 . . ?
Cl5 C50 Cl4 111.1(2) . . ?
Cl5 C50 Cl6 110.8(2) . . ?
Cl5 C50 D50 108.4 . . ?
Cl6 C50 D50 108.4 . . ?
Cl7 C51 Cl8 110.3(2) . . ?
Cl7 C51 D51 108.2 . . ?
Cl8 C51 D51 108.2 . . ?
Cl9 C51 Cl7 111.4(2) . . ?
Cl9 C51 Cl8 110.6(2) . . ?
Cl9 C51 D51 108.2 . . ?
Cl1 C49 Cl2 110.6(2) . . ?
Cl1 C49 Cl3 109.2(2) . . ?
Cl1 C49 D49 108.9 . . ?
Cl2 C49 Cl3 110.4(2) . . ?
Cl2 C49 D49 108.9 . . ?
Cl3 C49 D49 108.9 . . ?
Cl10 C52 D52 108.6 . . ?
Cl11 C52 Cl10 109.7(2) . . ?
Cl11 C52 D52 108.6 . . ?
Cl12 C52 Cl10 111.2(2) . . ?
Cl12 C52 Cl11 110.2(2) . . ?
Cl12 C52 D52 108.6 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C8 H8 F2 0.95 2.21 2.853(4) 123.8 . yes
C11 H11 O2 0.95 2.55 3.163(4) 122.1 2_566 yes
C11 H11 N3 0.95 2.60 3.179(4) 120.0 . yes
C28 H28 F4 0.95 2.25 2.878(4) 122.4 . yes
C31 H31 O1 0.95 2.51 3.114(4) 121.3 . yes
C46 H46 F1 0.95 2.56 3.237(4) 128.4 1_455 yes
C50 D50 F3 1.00 2.41 3.124(4) 127.5 . yes
C50 D50 N4 1.00 2.50 3.299(5) 136.8 1_455 yes
C49 D49 O2 1.00 2.18 3.021(4) 141.2 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ir O1 C41 O2 178.4(3) . . . . ?
Ir O1 C41 C42 -2.5(3) . . . . ?
Ir N1 C7 C6 0.6(3) . . . . ?
Ir N1 C7 C8 -176.0(2) . . . . ?
Ir N1 C11 C10 173.7(2) . . . . ?
Ir N2 C27 C26 -6.2(3) . . . . ?
Ir N2 C27 C28 173.0(2) . . . . ?
Ir N2 C31 C30 -173.1(2) . . . . ?
Ir N3 C42 C41 2.2(3) . . . . ?
Ir N3 C42 C43 -178.7(3) . . . . ?
Ir N3 C46 C45 179.5(2) . . . . ?
Ir C1 C2 C3 177.6(2) . . . . ?
Ir C1 C6 C5 -176.5(2) . . . . ?
Ir C1 C6 C7 6.4(3) . . . . ?
Ir C21 C22 C23 176.9(2) . . . . ?
Ir C21 C26 C25 -175.6(2) . . . . ?
Ir C21 C26 C27 4.5(3) . . . . ?
F1 C3 C4 C5 179.6(3) . . . . ?
F1 C3 C4 C47 -2.4(5) . . . . ?
F2 C5 C6 C1 178.3(3) . . . . ?
F2 C5 C6 C7 -4.9(5) . . . . ?
F3 C23 C24 C25 -178.7(3) . . . . ?
F3 C23 C24 C48 3.3(4) . . . . ?
F4 C25 C26 C21 177.1(3) . . . . ?
F4 C25 C26 C27 -3.0(5) . . . . ?
O1 C41 C42 N3 0.2(4) . . . . ?
O1 C41 C42 C43 -178.9(3) . . . . ?
O2 C41 C42 N3 179.4(3) . . . . ?
O2 C41 C42 C43 0.4(5) . . . . ?
N1 C7 C8 C9 2.6(5) . . . . ?
N2 C27 C28 C29 0.9(4) . . . . ?
N3 C42 C43 C44 -1.6(5) . . . . ?
C1 C2 C3 F1 179.9(3) . . . . ?
C1 C2 C3 C4 -1.3(5) . . . . ?
C1 C6 C7 N1 -4.6(4) . . . . ?
C1 C6 C7 C8 171.8(3) . . . . ?
C2 C1 C6 C5 1.2(4) . . . . ?
C2 C1 C6 C7 -175.9(3) . . . . ?
C2 C3 C4 C5 0.7(5) . . . . ?
C2 C3 C4 C47 178.8(3) . . . . ?
C3 C4 C5 F2 -179.3(3) . . . . ?
C3 C4 C5 C6 0.8(5) . . . . ?
C4 C5 C6 C1 -1.8(5) . . . . ?
C4 C5 C6 C7 175.0(3) . . . . ?
C5 C6 C7 N1 178.5(3) . . . . ?
C5 C6 C7 C8 -5.1(5) . . . . ?
C6 C1 C2 C3 0.3(5) . . . . ?
C6 C7 C8 C9 -173.5(3) . . . . ?
C7 N1 C11 C10 -0.2(5) . . . . ?
C7 C8 C9 C10 -1.8(5) . . . . ?
C7 C8 C9 C12B -176.6(5) . . . . ?
C7 C8 C9 C12A 170.9(4) . . . . ?
C8 C9 C10 C11 0.1(5) . . . . ?
C8 C9 C12B C13B 113.2(8) . . . . ?
C8 C9 C12B C17B -65.5(9) . . . . ?
C8 C9 C12A C13A 112.3(7) . . . . ?
C8 C9 C12A C17A -67.1(8) . . . . ?
C9 C10 C11 N1 0.9(5) . . . . ?
C9 C12B C13B C14B -177.4(7) . . . . ?
C9 C12B C13B C18B 4.7(13) . . . . ?
C9 C12B C17B C16B 178.6(7) . . . . ?
C9 C12B C17B C20B -5.9(12) . . . . ?
C9 C12A C13A C14A -178.8(6) . . . . ?
C9 C12A C13A C18A 1.0(11) . . . . ?
C9 C12A C17A C16A 178.1(6) . . . . ?
C9 C12A C17A C20A -4.7(11) . . . . ?
C10 C9 C12B C13B -61.5(10) . . . . ?
C10 C9 C12B C17B 119.8(7) . . . . ?
C10 C9 C12A C13A -75.5(8) . . . . ?
C10 C9 C12A C17A 105.1(7) . . . . ?
C11 N1 C7 C6 175.0(3) . . . . ?
C11 N1 C7 C8 -1.6(4) . . . . ?
C21 C22 C23 F3 179.8(3) . . . . ?
C21 C22 C23 C24 -1.1(5) . . . . ?
C21 C26 C27 N2 1.1(4) . . . . ?
C21 C26 C27 C28 -178.1(3) . . . . ?
C22 C21 C26 C25 2.9(4) . . . . ?
C22 C21 C26 C27 -176.9(3) . . . . ?
C22 C23 C24 C25 2.1(5) . . . . ?
C22 C23 C24 C48 -175.8(3) . . . . ?
C23 C24 C25 F4 -179.6(3) . . . . ?
C23 C24 C25 C26 -0.5(5) . . . . ?
C24 C25 C26 C21 -1.9(5) . . . . ?
C24 C25 C26 C27 177.9(3) . . . . ?
C25 C26 C27 N2 -178.7(3) . . . . ?
C25 C26 C27 C28 2.1(5) . . . . ?
C26 C21 C22 C23 -1.5(4) . . . . ?
C26 C27 C28 C29 -180.0(3) . . . . ?
C27 N2 C31 C30 2.3(5) . . . . ?
C27 C28 C29 C30 1.2(5) . . . . ?
C27 C28 C29 C32 -179.4(3) . . . . ?
C28 C29 C30 C31 -1.6(5) . . . . ?
C28 C29 C32 C33 69.3(4) . . . . ?
C28 C29 C32 C37 -111.4(3) . . . . ?
C29 C30 C31 N2 -0.2(5) . . . . ?
C29 C32 C33 C34 -179.2(3) . . . . ?
C29 C32 C33 C38 2.7(5) . . . . ?
C29 C32 C37 C36 177.9(3) . . . . ?
C29 C32 C37 C40 -3.1(5) . . . . ?
C30 C29 C32 C33 -111.3(4) . . . . ?
C30 C29 C32 C37 68.0(4) . . . . ?
C31 N2 C27 C26 178.1(3) . . . . ?
C31 N2 C27 C28 -2.6(4) . . . . ?
C32 C29 C30 C31 179.0(3) . . . . ?
C32 C33 C34 C35 1.1(5) . . . . ?
C33 C32 C37 C36 -2.8(5) . . . . ?
C33 C32 C37 C40 176.2(3) . . . . ?
C33 C34 C35 C36 -2.3(5) . . . . ?
C33 C34 C35 C39 177.4(3) . . . . ?
C34 C35 C36 C37 1.0(5) . . . . ?
C35 C36 C37 C32 1.5(5) . . . . ?
C35 C36 C37 C40 -177.4(3) . . . . ?
C37 C32 C33 C34 1.5(5) . . . . ?
C37 C32 C33 C38 -176.6(3) . . . . ?
C38 C33 C34 C35 179.2(3) . . . . ?
C39 C35 C36 C37 -178.8(3) . . . . ?
C41 C42 C43 C44 177.4(3) . . . . ?
C42 N3 C46 C45 -1.2(5) . . . . ?
C42 C43 C44 C45 0.6(6) . . . . ?
C43 C44 C45 C46 0.1(6) . . . . ?
C44 C45 C46 N3 0.2(5) . . . . ?
C46 N3 C42 C41 -177.1(3) . . . . ?
C46 N3 C42 C43 1.9(5) . . . . ?
C47 C4 C5 F2 2.7(5) . . . . ?
C47 C4 C5 C6 -177.2(3) . . . . ?
C48 C24 C25 F4 -1.7(4) . . . . ?
C48 C24 C25 C26 177.4(3) . . . . ?
C12B C9 C10 C11 174.9(5) . . . . ?
C12B C13B C14B C15B -1.3(14) . . . . ?
C13B C12B C17B C16B -0.1(13) . . . . ?
C13B C12B C17B C20B 175.4(8) . . . . ?
C13B C14B C15B C16B 0.2(18) . . . . ?
C13B C14B C15B C19B -179.0(11) . . . . ?
C14B C15B C16B C17B 0.9(18) . . . . ?
C15B C16B C17B C12B -1.0(14) . . . . ?
C15B C16B C17B C20B -176.7(10) . . . . ?
C17B C12B C13B C14B 1.2(13) . . . . ?
C17B C12B C13B C18B -176.7(8) . . . . ?
C18B C13B C14B C15B 176.7(10) . . . . ?
C19B C15B C16B C17B -179.8(11) . . . . ?
C12A C9 C10 C11 -172.2(5) . . . . ?
C12A C13A C14A C15A 1.0(13) . . . . ?
C13A C12A C17A C16A -1.3(11) . . . . ?
C13A C12A C17A C20A 175.9(7) . . . . ?
C13A C14A C15A C16A -1.8(15) . . . . ?
C13A C14A C15A C19A -178.6(10) . . . . ?
C14A C15A C16A C17A 1.1(15) . . . . ?
C15A C16A C17A C12A 0.5(12) . . . . ?
C15A C16A C17A C20A -176.8(8) . . . . ?
C17A C12A C13A C14A 0.6(12) . . . . ?
C17A C12A C13A C18A -179.6(7) . . . . ?
C18A C13A C14A C15A -178.8(9) . . . . ?
C19A C15A C16A C17A 177.9(10) . . . . ?
_shelx_res_file
;
TITL 19srv247_a.res in P-1
19srv248.res
created by SHELXL-2018/3 at 17:59:52 on 14-Nov-2019
REM Old TITL 19srv247 in P1
REM SHELXT solution in P-1: R1 0.119, Rweak 0.014, Alpha 0.090
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C52 N6 O F16 Ir
CELL 0.71073 10.0759 16.3073 17.9412 89.3872 76.798 89.1792
ZERR 2 0.0005 0.0008 0.0008 0.0015 0.0014 0.0015
LATT 1
SFAC C H Cl D F Ir N O
UNIT 104 68 24 8 8 2 10 4
EQIV $1 -1+X,+Y,+Z
EQIV $2 -X,1-Y,1-Z
SIMU 0.04 0.08 1
L.S. 7
PLAN 10
SIZE 0.059 0.08 0.096
TEMP -153.15
HTAB C46 F1_$1
HTAB C8 F2
HTAB C11 O2_$2
HTAB C11 N3
HTAB C28 F4
HTAB C31 O1
HTAB C49 O2
HTAB C50 F3
HTAB C50 N4_$1
BOND
list 4
fmap 2 53
acta 57
MORE -1
BOND $H
CONF
OMIT 2 4 1
OMIT 0 -2 5
REM
REM
REM
WGHT 0.039800
FVAR 0.10318 0.03347 0.04553 0.45811
IR 6 0.186049 0.266037 0.453906 11.00000 0.01345 0.00833 =
0.01052 0.00360 -0.00281 -0.00049
F1 5 0.699524 0.143572 0.414996 11.00000 0.01869 0.02455 =
0.02633 0.00703 -0.01054 0.00577
F2 5 0.584809 0.278346 0.207617 11.00000 0.02079 0.03119 =
0.01312 0.00661 0.00116 0.00773
F3 5 0.064517 0.032237 0.271037 11.00000 0.04765 0.01907 =
0.01587 0.00021 -0.01852 -0.00395
F4 5 0.175983 -0.052120 0.498129 11.00000 0.03017 0.01038 =
0.01610 0.00495 -0.01185 0.00031
O1 8 0.210760 0.383071 0.502374 11.00000 0.01605 0.01098 =
0.01756 0.00116 -0.00270 -0.00153
O2 8 0.097398 0.484122 0.573545 11.00000 0.02437 0.01784 =
0.03192 -0.01123 -0.00630 0.00354
N1 7 0.192381 0.326327 0.352565 11.00000 0.01495 0.00920 =
0.01241 0.00492 -0.00398 -0.00213
N2 7 0.202522 0.201250 0.548881 11.00000 0.01395 0.01284 =
0.00955 0.00004 -0.00197 -0.00087
N3 7 -0.017336 0.301835 0.505455 11.00000 0.01595 0.01289 =
0.01337 0.00434 -0.00271 -0.00024
N4 7 0.888805 0.188175 0.230130 11.00000 0.02381 0.03930 =
0.03126 0.00548 -0.00216 0.00850
N5 7 0.109910 -0.163420 0.347745 11.00000 0.02914 0.01898 =
0.01710 -0.00015 -0.00451 -0.00005
C1 1 0.379666 0.242183 0.401698 11.00000 0.01503 0.00671 =
0.01489 0.00271 -0.00418 0.00009
C2 1 0.477863 0.198915 0.430785 11.00000 0.01802 0.01592 =
0.01106 0.00459 -0.00435 0.00057
AFIX 43
H2 2 0.455764 0.178754 0.481947 11.00000 -1.20000
AFIX 0
C3 1 0.605054 0.185504 0.386174 11.00000 0.01858 0.01115 =
0.02037 0.00328 -0.01141 0.00279
C4 1 0.644186 0.211721 0.310327 11.00000 0.01513 0.01295 =
0.01845 0.00090 -0.00361 0.00089
C5 1 0.545700 0.254153 0.281563 11.00000 0.01901 0.01259 =
0.01181 0.00170 -0.00227 0.00109
C6 1 0.416610 0.271082 0.324664 11.00000 0.01323 0.01182 =
0.01653 0.00243 -0.00619 0.00049
C7 1 0.312925 0.320785 0.299234 11.00000 0.01559 0.00863 =
0.01165 0.00245 -0.00190 -0.00084
C8 1 0.329886 0.363872 0.230511 11.00000 0.01810 0.01467 =
0.01204 0.00177 -0.00377 0.00180
AFIX 43
H8 2 0.412647 0.357842 0.192896 11.00000 -1.20000
AFIX 0
C9 1 0.227560 0.415781 0.215820 11.00000 0.01939 0.01102 =
0.01488 0.00257 -0.00460 -0.00161
C10 1 0.106455 0.420946 0.271579 11.00000 0.02186 0.01207 =
0.02036 0.00441 -0.00778 0.00298
AFIX 43
H10 2 0.033943 0.455500 0.263930 11.00000 -1.20000
AFIX 0
C11 1 0.092814 0.375247 0.338222 11.00000 0.01354 0.01342 =
0.01859 0.00450 -0.00336 -0.00062
AFIX 43
H11 2 0.009196 0.378651 0.375511 11.00000 -1.20000
AFIX 0
C21 1 0.150287 0.154365 0.420395 11.00000 0.00929 0.01304 =
0.01218 0.00060 -0.00198 0.00176
C22 1 0.114185 0.133412 0.352152 11.00000 0.01932 0.01559 =
0.01436 0.00629 -0.00593 -0.00098
AFIX 43
H22 2 0.099976 0.175023 0.317234 11.00000 -1.20000
AFIX 0
C23 1 0.099567 0.052846 0.336173 11.00000 0.01766 0.02156 =
0.00918 0.00064 -0.00527 -0.00133
C24 1 0.121111 -0.011354 0.384264 11.00000 0.01427 0.01008 =
0.01473 0.00059 -0.00329 -0.00124
C25 1 0.154644 0.010427 0.452308 11.00000 0.01431 0.01196 =
0.01353 0.00638 -0.00417 0.00080
C26 1 0.167745 0.090892 0.472331 11.00000 0.01189 0.01338 =
0.00998 -0.00031 -0.00305 -0.00141
C27 1 0.198608 0.117962 0.544457 11.00000 0.01218 0.01131 =
0.01122 0.00096 -0.00247 -0.00172
C28 1 0.223986 0.069256 0.603941 11.00000 0.01576 0.01134 =
0.01247 0.00224 -0.00386 -0.00068
AFIX 43
H28 2 0.222391 0.011229 0.600193 11.00000 -1.20000
AFIX 0
C29 1 0.251738 0.104777 0.669002 11.00000 0.01357 0.01448 =
0.01420 0.00128 -0.00337 0.00036
C30 1 0.250456 0.190066 0.672643 11.00000 0.02489 0.01676 =
0.01346 -0.00017 -0.00870 -0.00199
AFIX 43
H30 2 0.266644 0.216536 0.716585 11.00000 -1.20000
AFIX 0
C31 1 0.225612 0.235795 0.612242 11.00000 0.02536 0.01066 =
0.01561 0.00039 -0.00919 -0.00194
AFIX 43
H31 2 0.224774 0.293914 0.615511 11.00000 -1.20000
AFIX 0
C32 1 0.280250 0.052369 0.732219 11.00000 0.02236 0.01135 =
0.01358 0.00043 -0.00885 -0.00038
C33 1 0.401588 0.006238 0.720856 11.00000 0.02160 0.01754 =
0.01490 -0.00094 -0.00705 -0.00047
C34 1 0.425215 -0.043064 0.780451 11.00000 0.02834 0.02249 =
0.02486 -0.00144 -0.01317 0.00752
AFIX 43
H34 2 0.508090 -0.073630 0.773193 11.00000 -1.20000
AFIX 0
C35 1 0.331587 -0.048899 0.849978 11.00000 0.04090 0.01896 =
0.01627 0.00358 -0.01468 0.00276
C36 1 0.213990 -0.001815 0.860518 11.00000 0.03130 0.02011 =
0.01317 0.00041 -0.00325 -0.00273
AFIX 43
H36 2 0.149789 -0.004762 0.908304 11.00000 -1.20000
AFIX 0
C37 1 0.186029 0.050025 0.803395 11.00000 0.02409 0.01412 =
0.01400 0.00159 -0.00812 -0.00401
C38 1 0.507972 0.010909 0.646928 11.00000 0.02151 0.02576 =
0.02536 -0.00122 -0.00405 0.00368
AFIX 137
H38A 2 0.581912 -0.028270 0.648615 11.00000 31.00000
H38B 2 0.544576 0.066524 0.639840 11.00000 31.00000
H38C 2 0.466705 -0.002485 0.604189 11.00000 31.00000
AFIX 0
C39 1 0.356982 -0.105379 0.912428 11.00000 0.06787 0.03425 =
0.02415 0.00795 -0.01563 0.01681
AFIX 123
H39A 2 0.444881 -0.133683 0.894923 10.50000 -1.50000
H39B 2 0.358454 -0.073320 0.958117 10.50000 -1.50000
H39C 2 0.284125 -0.145861 0.924854 10.50000 -1.50000
H39D 2 0.280093 -0.101560 0.957006 10.50000 -1.50000
H39E 2 0.366519 -0.161923 0.893813 10.50000 -1.50000
H39F 2 0.440849 -0.089382 0.927076 10.50000 -1.50000
AFIX 0
C40 1 0.058659 0.102300 0.819943 11.00000 0.02425 0.02043 =
0.01836 0.00053 -0.00316 0.00058
AFIX 137
H40A 2 0.081016 0.157920 0.832772 11.00000 21.00000
H40B 2 -0.007646 0.078669 0.863160 11.00000 21.00000
H40C 2 0.019611 0.104375 0.774679 11.00000 21.00000
AFIX 0
C41 1 0.102101 0.417909 0.540483 11.00000 0.01834 0.01656 =
0.01517 0.00269 -0.00351 -0.00067
C42 1 -0.029746 0.373792 0.543545 11.00000 0.01773 0.01452 =
0.01611 0.00159 -0.00312 -0.00011
C43 1 -0.154619 0.404244 0.581082 11.00000 0.02575 0.02344 =
0.03257 -0.00922 -0.00339 0.00163
AFIX 43
H43 2 -0.160906 0.454151 0.608574 11.00000 -1.20000
AFIX 0
C44 1 -0.270913 0.361716 0.578522 11.00000 0.01653 0.03199 =
0.04133 -0.00648 0.00159 0.00292
AFIX 43
H44 2 -0.358250 0.382082 0.603752 11.00000 -1.20000
AFIX 0
C45 1 -0.258058 0.289570 0.538910 11.00000 0.01541 0.02884 =
0.03448 -0.00127 -0.00482 -0.00361
AFIX 43
H45 2 -0.336784 0.259355 0.536343 11.00000 -1.20000
AFIX 0
C46 1 -0.130922 0.261161 0.502960 11.00000 0.02147 0.01600 =
0.02085 0.00337 -0.00730 -0.00409
AFIX 43
H46 2 -0.123170 0.211182 0.475486 11.00000 -1.20000
AFIX 0
C47 1 0.779846 0.198066 0.265176 11.00000 0.02195 0.02397 =
0.02079 0.00103 -0.00727 0.00550
C48 1 0.113819 -0.096197 0.363948 11.00000 0.01628 0.02065 =
0.00919 0.00265 -0.00507 0.00231
PART 1
C12B 1 0.242619 0.457768 0.141622 41.00000 0.01159
C13B 1 0.161581 0.440617 0.089621 41.00000 0.01673
C14B 1 0.189019 0.481937 0.019912 41.00000 0.01691
AFIX 43
H14B 2 0.136222 0.470100 -0.016179 41.00000 -1.20000
AFIX 0
C15B 1 0.289644 0.539251 0.001273 41.00000 0.01845 0.03557 =
0.01657 0.00670 -0.00064 0.00427
C16B 1 0.368381 0.557596 0.052486 41.00000 0.01956
AFIX 43
H16B 2 0.437129 0.597940 0.039716 41.00000 -1.20000
AFIX 0
C17B 1 0.346687 0.516339 0.123928 41.00000 0.01732
C18B 1 0.046184 0.382129 0.108880 41.00000 0.02203
AFIX 3
H18A 2 0.025104 0.362849 0.061380 41.00000 -1.50000
H18B 2 -0.034286 0.409599 0.140170 41.00000 -1.50000
H18C 2 0.072154 0.335279 0.137360 41.00000 -1.50000
AFIX 0
C19B 1 0.315967 0.584808 -0.075506 41.00000 0.03632 0.06523 =
0.02411 0.02864 0.01810 0.01454
AFIX 3
H19A 2 0.401277 0.615118 -0.082586 41.00000 -1.50000
H19B 2 0.240537 0.623288 -0.075936 41.00000 -1.50000
H19C 2 0.323107 0.545398 -0.117136 41.00000 -1.50000
AFIX 0
C20B 1 0.430051 0.541776 0.179628 41.00000 0.02389
AFIX 3
H20A 2 0.495031 0.583986 0.156158 41.00000 -1.50000
H20B 2 0.479821 0.493996 0.193358 41.00000 -1.50000
H20C 2 0.368981 0.563756 0.225798 41.00000 -1.50000
AFIX 0
SAME 0.02 0.04 C12B > C20B
PART 0
PART 2
C12A 1 0.261202 0.470132 0.145413 -41.00000 0.01309
C13A 1 0.196153 0.453678 0.085472 -41.00000 0.01979
C14A 1 0.228835 0.502927 0.019017 -41.00000 0.02103
AFIX 43
H14A 2 0.185196 0.493467 -0.021721 -41.00000 -1.20000
AFIX 0
C15A 1 0.322218 0.564076 0.012125 -41.00000 0.02164 0.02672 =
0.02054 0.00197 -0.00122 0.00817
C16A 1 0.383494 0.579912 0.071930 -41.00000 0.02368
AFIX 43
H16A 2 0.447083 0.623215 0.066897 -41.00000 -1.20000
AFIX 0
C17A 1 0.354044 0.533704 0.139560 -41.00000 0.01689
C18A 1 0.093930 0.385702 0.089373 -41.00000 0.03250
AFIX 3
H18D 2 0.082730 0.374522 0.037613 -41.00000 -1.50000
H18E 2 0.005920 0.402282 0.121913 -41.00000 -1.50000
H18F 2 0.127510 0.336082 0.110713 -41.00000 -1.50000
AFIX 0
C19A 1 0.352695 0.617798 -0.060656 -41.00000 0.05171 0.06121 =
0.02802 0.02986 0.00725 0.01112
AFIX 3
H19D 2 0.440375 0.644898 -0.065046 -41.00000 -1.50000
H19E 2 0.280405 0.659348 -0.057386 -41.00000 -1.50000
H19F 2 0.356795 0.583618 -0.105746 -41.00000 -1.50000
AFIX 0
C20A 1 0.416300 0.555171 0.204353 -41.00000 0.02347
AFIX 3
H20D 2 0.344730 0.557561 0.251583 -41.00000 -1.50000
H20E 2 0.460260 0.608671 0.194583 -41.00000 -1.50000
H20F 2 0.484290 0.513321 0.209793 -41.00000 -1.50000
AFIX 0
PART 0
CL4 3 0.258044 0.192101 0.143896 11.00000 0.04680 0.03552 =
0.04618 -0.00847 -0.01236 0.00025
CL5 3 0.114113 0.148691 0.028286 11.00000 0.08207 0.05720 =
0.02632 0.00653 -0.01684 -0.00549
CL6 3 0.260567 0.024879 0.094390 11.00000 0.05077 0.02802 =
0.06371 -0.00532 0.00969 0.00535
C50 1 0.163972 0.116237 0.111054 11.00000 0.03978 0.02682 =
0.02191 0.00025 -0.00195 0.00270
AFIX 13
D50 4 0.080071 0.105415 0.151829 11.00000 -1.20000
AFIX 0
CL7 3 0.527898 0.163118 0.929873 11.00000 0.09493 0.09524 =
0.06053 -0.00562 -0.05301 0.03386
CL8 3 0.339896 0.252554 0.860459 11.00000 0.03724 0.03631 =
0.03779 0.00185 -0.01312 -0.00045
CL9 3 0.588373 0.187585 0.766744 11.00000 0.04815 0.07617 =
0.05487 -0.02172 0.01413 -0.01943
C51 1 0.460709 0.172370 0.848969 11.00000 0.03463 0.02946 =
0.03584 0.00072 -0.01394 0.00016
AFIX 13
D51 4 0.413476 0.120134 0.843052 11.00000 -1.20000
AFIX 0
CL1 3 0.267408 0.582254 0.696731 11.00000 0.03058 0.03946 =
0.09569 -0.03484 0.01313 -0.00815
CL2 3 0.518108 0.554305 0.582960 11.00000 0.02697 0.03243 =
0.04180 -0.00795 -0.00312 -0.01143
CL3 3 0.373359 0.418265 0.668367 11.00000 0.02704 0.03245 =
0.05546 -0.00308 -0.00239 -0.00692
C49 1 0.356408 0.514928 0.626150 11.00000 0.02128 0.02681 =
0.04932 -0.01288 -0.00454 -0.00604
AFIX 13
D49 4 0.302970 0.508519 0.586004 11.00000 -1.20000
AFIX 0
CL10 3 0.061446 0.713382 0.070258 11.00000 0.09027 0.03502 =
0.02856 0.00000 -0.01441 0.02461
CL11 3 -0.101288 0.596841 0.171072 11.00000 0.03451 0.06068 =
0.08910 -0.00490 -0.00468 0.00040
CL12 3 0.085600 0.697185 0.227141 11.00000 0.07268 0.04842 =
0.03757 -0.01001 -0.02961 0.01643
C52 1 0.056835 0.645737 0.147659 11.00000 0.03619 0.02197 =
0.02923 0.00003 -0.00693 0.00676
AFIX 13
D52 4 0.129997 0.603134 0.131978 11.00000 -1.20000
AFIX 0
HKLF 4
REM 19srv247_a.res in P-1
REM wR2 = 0.0774, GooF = S = 0.983, Restrained GooF = 0.982 for all data
REM R1 = 0.0361 for 12529 Fo > 4sig(Fo) and 0.0547 for all 15449 data
REM 701 parameters refined using 52 restraints
END
WGHT 0.0398 0.0000
REM Highest difference peak 2.192, deepest hole -1.365, 1-sigma level 0.133
Q1 1 0.2621 0.2767 0.4607 11.00000 0.05 2.19
Q2 1 0.0976 0.2604 0.4526 11.00000 0.05 1.83
Q3 1 0.2247 0.2362 0.4187 11.00000 0.05 1.81
Q4 1 0.1433 0.3002 0.4857 11.00000 0.05 1.51
Q5 1 0.6058 0.1790 0.8919 11.00000 0.05 0.95
Q6 1 0.1466 0.2266 0.4208 11.00000 0.05 0.79
Q7 1 0.1464 0.7310 0.0840 11.00000 0.05 0.73
Q8 1 -0.1059 0.6379 0.1354 11.00000 0.05 0.69
Q9 1 -0.0808 0.3015 0.5005 11.00000 0.05 0.62
Q10 1 0.5668 0.2217 0.7345 11.00000 0.05 0.61
;
_shelx_res_checksum 8449
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: d-chloroform'
_exptl_crystal_preparation Luminescent